pH Meter pH 960 - Precisa Gravimetrics AG

pH Meter pH 960 - Precisa Gravimetrics AG
Precisa
pH960
Precisa
pH Meter
pH 960
Operating Instructions
350-8110-000a
Precisa Instruments AG
Moosmattstrasse 32
CH-8953 Dietikon/Switzerland
Internet
www.precisa.com
pH Meter pH960
Instructions for Use
Copyright
These operating instructions are protected by copyright. All rights reserved. No part of the operating instructions may be reproduced, processed, duplicated or published in any form by photocopying, microfilming, reprinting or other process, in
particular electronic means, without the written agreement of Precisa Instruments AG
© Precisa Instruments AG, 8953 Dietikon, Switzerland, 2004
350-8110-000a
01.2004
Contents
Contents
1 Introduction.......................................................... 1
1.1
Instrument description.................................................................................2
1.2
Parts and controls........................................................................................3
1.3
Information about these Instructions for Use .............................................5
1.3.1
Organization............................................................................................. 5
1.3.2
Notation and pictograms......................................................................... 6
1.4
Safety information ........................................................................................7
1.4.1
Electrical safety ........................................................................................ 7
1.4.2
General handling rules ............................................................................ 7
2 Installation ........................................................... 8
2.1
2.2
Instrument setup ..........................................................................................8
2.1.1
Packaging ................................................................................................ 8
2.1.2
Checks ..................................................................................................... 8
2.1.3
Location ................................................................................................... 8
Connecting the accessories ........................................................................9
2.2.1
Connecting the 101 Magnetic Stirrer..................................................... 11
2.3
Connecting optional devices .....................................................................12
2.3.1
Connecting a printer .............................................................................. 12
2.4
Connecting the electrodes and sensors ...................................................14
2.5
Mains connection .......................................................................................15
2.6
Switch on....................................................................................................15
2.7
Initial configuration ....................................................................................16
3 Short operating tutorial ..................................... 17
3.1
pH measurement........................................................................................17
3.1.1
Requirements......................................................................................... 17
3.1.2
Preparations........................................................................................... 17
3.1.3
pH calibration......................................................................................... 18
3.1.4
pH measurement ................................................................................... 20
4 Operation ........................................................... 21
4.1
The keypad .................................................................................................21
4.2
Operating concept .....................................................................................22
4.3
All key functions at a glance......................................................................23
4.4
Operating principles ..................................................................................28
4.4.1
Configuration and method parameters ................................................. 28
4.4.2
Editing menu entries.............................................................................. 29
4.4.3
Entering text ........................................................................................... 30
5 Configuration ..................................................... 31
5.1
Report.........................................................................................................32
5.2
Printing out measured values....................................................................34
5.3
Storing measured values ...........................................................................37
5.4
Auxiliaries...................................................................................................37
5.5
Monitoring ..................................................................................................41
I
Contents
5.6
Peripheral units.......................................................................................... 42
5.7
RS 232 settings .......................................................................................... 43
6 Methods / Parameters........................................ 44
6.1
6.2
Method management ................................................................................. 44
pH measurement (pH mode) ..................................................................... 45
6.2.1
Measuring parameters .......................................................................... 45
6.2.2
Calibration parameters .......................................................................... 47
6.2.3
Limits pH................................................................................................ 50
6.2.4
Limits T .................................................................................................. 51
6.2.5
Plot parameters ..................................................................................... 51
6.2.6
Preselections ......................................................................................... 52
6.2.7
Electrode test......................................................................................... 53
6.3
Temperature measurement (T mode)........................................................ 54
6.3.1
Measuring parameters .......................................................................... 54
6.3.2
Limits T .................................................................................................. 55
6.3.3
Plot parameters ..................................................................................... 56
6.3.4
Preselections ......................................................................................... 56
6.4
Potential measurement (U mode).............................................................. 57
6.4.1
Measuring parameters .......................................................................... 57
6.4.2
Limits U.................................................................................................. 58
6.4.3
Plot parameters ..................................................................................... 59
6.4.4
Preselections ......................................................................................... 59
7 Various functions ............................................... 60
II
7.1
Calibration data.......................................................................................... 60
7.1.1
pH calibration data ................................................................................ 61
7.2
Reports....................................................................................................... 65
7.2.1
Arrangement of a report ........................................................................ 67
7.2.2
Report identification............................................................................... 68
7.2.3
Measuring point report .......................................................................... 68
7.2.4
Calibration report................................................................................... 70
7.2.5
Configuration report .............................................................................. 70
7.2.6
Parameter report.................................................................................... 72
7.2.7
Measured values memory report .......................................................... 73
7.2.8
User method report ............................................................................... 74
7.3
Measured values memory ......................................................................... 75
7.3.1
Save measured values .......................................................................... 75
7.3.2
Print measured values........................................................................... 75
7.3.3
Show measured values ......................................................................... 76
7.4
Limit monitoring ......................................................................................... 77
7.4.1
Uses....................................................................................................... 77
7.4.2
How it functions ..................................................................................... 78
7.5
Setup .......................................................................................................... 79
7.5.1
Locking .................................................................................................. 79
7.5.2
Input assignment................................................................................... 80
7.5.3
Graphics ................................................................................................ 80
Contents
8 Troubleshooting – Messages – Maintenance .... 81
8.1
Troubleshooting .........................................................................................81
8.2
Messages ...................................................................................................82
8.3
8.4
QM support ................................................................................................88
Validation....................................................................................................90
8.4.1
Electronic tests ...................................................................................... 90
8.4.2
Wet tests ................................................................................................ 91
8.4.3
pH Meter maintenance .......................................................................... 91
8.5
Diagnosis....................................................................................................92
8.6
Checking the measuring input ..................................................................94
8.7
pH electrode test........................................................................................97
8.7.1
Preparations........................................................................................... 97
8.7.2
Procedure .............................................................................................. 98
8.7.3
Results ................................................................................................. 100
8.7.4
Messages and measures .................................................................... 102
8.7.5
Care and maintenance of pH glass electrodes .................................. 103
9 Annex................................................................ 105
9.1
Technical data ..........................................................................................105
9.1.1
Measuring modes................................................................................ 105
9.1.2
Measuring inputs ................................................................................. 105
9.1.3
Measuring input specifications............................................................ 106
9.1.4
Interfaces ............................................................................................. 106
9.1.5
Power supply ....................................................................................... 106
9.1.6
Safety specifications............................................................................ 107
9.1.7
Electromagnetic compatibility (EMC).................................................. 107
9.1.8
Ambient temperature ........................................................................... 107
9.1.9
Reference conditions........................................................................... 107
9.1.10 Dimensions .......................................................................................... 107
9.2
Evaluation.................................................................................................108
9.2.1
pH calibration....................................................................................... 108
9.3
Menu structures .......................................................................................112
9.3.1
Instrument configuration...................................................................... 112
9.3.2
Method parameters in the pH mode ................................................... 114
9.3.3
Method parameters in the T mode...................................................... 115
9.3.4
Method parameters in the U mode ..................................................... 115
9.4
Stored buffer series .................................................................................116
9.5
Standard equipment.................................................................................120
9.5.1
pH960 pH Meter .................................................................................. 120
9.6
Optional accessories ...............................................................................122
9.6.1
Various ................................................................................................. 122
9.6.2
Connections......................................................................................... 122
9.7
Warranty and conformity .........................................................................123
9.7.1
Warranty ............................................................................................... 123
9.7.2
EU Declaration of Conformity for pH960 pH Meter............................. 123
9.7.3
Certificate of Conformity and System Validation: pH960 pH Meter ... 125
III
Contents
List of illustrations
Fig. 1:
Fig. 2:
Fig. 3:
Fig. 4:
Fig. 5:
Fig. 6:
Fig. 7:
Fig. 8:
Fig. 9:
Fig. 10:
IV
pH Meter pH960 connected to 101 Magnetic Stirrer............................................1
Front view of the pH Meter pH960 ........................................................................3
Rear view of the pH Meter pH960 .........................................................................4
Possible arrangements for mounting the base plate. ..........................................9
Attaching the support rod and base plate. .........................................................10
Ready-mounted pH measuring system ..............................................................11
Remote outputs in limit monitoring. ....................................................................78
Diagram showing changes in potential during an electrode test ....................100
Theoretical U/pH relationship............................................................................108
3-Point pH calibration ........................................................................................109
1 Introduction
1 Introduction
These instructions provide you with a comprehensive overview of the installation, working principles and operation of the pH960 pH Meter
Fig. 1:
pH Meter pH960 connected to 101 Magnetic Stirrer.
1
1 Introduction
1.1 Instrument description
The pH Meter pH960 is used for measuring pH, temperature and potential
reliably and at high resolution.
The pH Meter has comprehensive monitoring functions (for calibration, validation and service intervals), diagnostic functions and an automatic pH electrode test. Up to 100 values can be stored in the memory together with the
most important additional data; these can be viewed and outputted as a report. All the parameter settings for a measuring mode can be permanently
stored as a method.
All stored information (measured values, configuration, parameters, etc.) can
be transmitted via the RS 232 interface to a printer or computer for output as
a report.
The instrument has the following features:
• Dot-matrix display for both the continuous display of the measured value
and for showing the user dialog.
• High-impedance measuring input for pH, redox or ISE sensors, a connection for a separate reference electrode and an input for temperature sensors (Pt1000 or NTC).
• MSB connection (Serial Bus) for a stirrer.
• RS 232 connection for a serial printer or a computer.
• A connection for an external keyboard or a barcode reader.
2
1 Introduction
1.2 Parts and controls
Fig. 2:
Front view of the pH Meter pH960
1
LCD display
3
Main function keys
2
On/Off key
Key for switching the instrument on and
off
4
Input, navigation and
function keys
Each key has several functions;
the particular function depends on the
work status of the instrument
3
1 Introduction
Fig. 3:
4
Rear view of the pH Meter pH960
5
Connection for potentiometric electrodes
pH, ISE, redox or silver electrodes
with built-in or separate reference electrode; socket type F
10
RS232 interface
Connection for printer or PC
6
Connection for separate reference
electrode
4 mm socket type B
11
Barcode reader/
Keyboard connection
7
Serial number
12
12V power connection
8
Connection for temperature sensor
Pt1000 or NTC, for connection with two 2
mm B-plugs
13
Grounding connection
For measurements in grounded solutions, grounding of the instrument
may be advantageous to avoid interferences; 4 mm socket type B
9
MSB connection
(Serial Bus) for connecting a stirrer.
1 Introduction
1.3 Information about these Instructions for Use
Please study these instructions carefully before you start to use the pH
Meter pH960. The instructions contain information and warnings that
must be observed by the user in order to guarantee the safe use of
the instrument.
1.3.1 Organization
These Instructions for Use for the pH Meter pH960 provide a comprehensive overview about the installation, start-up, operation, troubleshooting and
technical specifications of the instruments. They are arranged as follows:
Sect. 1 Introduction
General description of the instrument and controls; safety information
Sect. 2 Installation
Installation of the instrument and accessories and start-up
Sect. 3 Short operating tutorial
Introduction to the operation by using two examples
Sect. 4 Operation
Detailed description of the operation
Sect. 5 Configuration
Detailed description of the instrument configuration
Sect. 6 Methods / Parameters
Description of all mode-specific parameters
Sect. 7 Various functions
Description of particular functions (calibration and addition data,
report output, measured value memory, limit monitoring)
Sect. 8 Troubleshooting – Messages – Maintenance
Information about instrument handling, maintenance and a description of possible errors and their remedies;
description of the GLP functions, support for system validation, diagnostic functions and pH electrode test
Sect. 9 Annex
Technical data, explanation of the evaluation calculations, menu
structures, stored buffer data, standard equipment,
optional accessories, warranty and conformity declarations
Index
In order to find the information you require about the pH Meter you should either use the Contents or the Index.
5
1 Introduction
1.3.2 Notation and pictograms
The following notations and pictograms (symbols) are used in these instructions:
Range
<MODE>
12
Menu item, parameter or input value
Key
Operating element
Danger
This symbol indicates a possible risk of death
or injury if the given information is not properly
observed.
Warning
This symbol indicates a possible risk of damage to the instrument or its components if the
given information is not properly observed.
Attention
This symbol indicates important information.
Please read it carefully before you continue.
Information
This symbol indicates additional information
and tips.
TIP !
6
TIP
This symbol indicates information that may be
of particular use to you.
1 Introduction
1.4 Safety information
Warning!
This instrument should only be used in accordance with the information given in these installation instructions.
1.4.1 Electrical safety
Please observe the following guidelines:
•
Only qualified Precisa technicians should carry out service work on electronic components.
•
Do not open the pH Meter housing. This could destroy the pH Meter. Inside the housing there are no components that the user can service or exchange.
Electrical safety when handling the pH Meter pH960 is guaranteed within the
framework of the IEC 61010 Standard. The following points must be observed:
Please make sure that the external power supply is always kept dry.
Protect it against direct liquid contact .
Electronic components are sensitive to electrostatic charges and can
be destroyed by a discharge. Always switch off the pH Meter before
making or breaking electrical connections on the rear panel of the instrument.
1.4.2 General handling rules
Handling solutions
When working with water or other solutions in the immediate vicinity of
the pH Meter please avoid excessive liquid splashes on the instrument housing or power supply. Any such splashes must be removed
as quickly as possible in order to prevent the liquid from entering the
instrument or the power supply.
7
2 Installation
2 Installation
2.1 Instrument setup
2.1.1 Packaging
The pH Meter pH960 and its specially packed accessories are supplied in
very protective special packaging made of shock absorbing polypropylene
foam. Please store this packaging in a safe place; it is the only way in which
the safe transport of the instrument can be guaranteed. Should you wish to
dispose of it please consider suitable disposal or recycling processes.
2.1.2 Checks
Please check that the delivery is complete and undamaged immediately on
receipt (compare with delivery note and list of accessories given in Section
9.5). If transport damage is evident please refer to the information given in
Section 9.7.1.
2.1.3 Location
Place the instrument on a suitable vibration-free laboratory bench, protected
from corrosive atmospheres and contact with chemicals.
8
2 Installation
2.2 Connecting the accessories
Both the stand for attaching the stirrer, clamping ring and electrode holder as
well as the pH Meter itself can be mounted on the supplied stand base.
You can chose between the arrangements shown in Fig. 4 to suit your own
particular working preference.
Fig. 4:
Possible arrangements for mounting the base plate.
Versions A and B are intended for mounting an 101 Magnetic Stirrer on the
left- and right-hand side of the pH Meter respectively. If you frequently work
without such a permanently attached stirrer then you can mount the base
plate so that you have space for the sample vessel directly in front of the
support rod (versions C and D).
9
2 Installation
Attach the base plate with the screws provided as shown in Fig. 5. The rubber
feet included prevent the system from slipping about on the work bench and
should therefore be stuck on to the base plate.
Fig. 5:
10
Attaching the support rod and base plate.
2 Installation
2.2.1 Connecting the 101 Magnetic Stirrer
Mount the magnetic stirrer on the support rod before attaching the clamping
ring (PN 3900-053) and the electrode holder (PN 3900-050). Further details
are given in the corresponding Instructions for Use.
For example, the ready-mounted system could look like this:
Fig. 6:
Ready-mounted pH measuring system
The 101 Magnetic Stirrer is controlled via MSB connection 9. The stirrer is
connected to it directly:
11
2 Installation
2.3 Connecting optional devices
Devices which are to be remotely controlled from the pH Meter.
2.3.1 Connecting a printer
A printer with a serial or parallel interface can be connected to the RS232 interface for printing out reports. The report output via the RS232 interface can
be made to either a printer or a PC.
The connection of the 40-character Custom DP40-S4N printer with the serial
Cable is described as an example:
The transmission parameters for the pH Meter and the printer must be the
same. On the pH Meter these are set under
CONFIG/peripheral units/character set: (see Sect. 5.6)
and under
CONFIG/RS232 settings (see Sect. 5.7).
These settings and other possible printer connections are given in the following table. If you wish to connect a printer which is not mentioned here then
make sure that it emulates the Epson mode or uses the international character set according to IBM Standard Table 437 and IBM-compatible graphics
control characters.
Please observe the paper feed settings after each report printout (see Sect.
5.1).
The settings for graph sizes in the printer output are accessible in the setup of
the pH Meter and are described in Sect.7.5.3. This can particularly be necessary for single sheet printers (i.e. HP Desk Jet).
12
2 Installation
Printer
Custom
DP40-S4N
Seiko
DPU-414
Cable
PN
121
PN
121
pH960 settings
3900- Character Set:
Baud Rate:
Data Bit:
Stop Bit:
Parity:
Handshake:
3900- Character Set:
Baud Rate:
Data Bit:
Stop Bit:
Parity:
Handshake:
Citizen
PN 3900- Character Set:
120
iDP562 RS
Baud Rate:
Data Bit:
Stop Bit:
Parity:
Handshake:
Epson LXPN 3900- As above, but
300+
120
Character Set:
HP Desk Jet PN 3900- Character Set:
with serial in- 120
Baud Rate:
terface
Data Bit:
Stop Bit:
Parity:
Handshake:
HP Desk Jet PN 3900- Character Set:
with parallel 116 RS232/ Baud Rate:
interface
Parallel
Data Bit:
Converter Stop Bit:
Parity:
Handshake:
Citizen
9600
8
1
none
HWs
Seiko
9600
8
1
none
HWs
Citizen
9600
8
1
none
HWs
Printer settings
IDP-560 EMULATION
FONT MAP = ENGLAND *
PRINT = REVERSE
LITTLE
CR CODE = VOID
CR AFTER B. FULL = VOID
CR ON B. EMPTY = VALID
BUFFER 1K BYTE
BAUD RATE = 9600
PROTOCOL = 8,N,1
FLOW CONTROL CTS-RTS
(*) FRANCE also for Italian, Spanish
and Portuguese,
GERMANY also for Swedish.
none
ON
1
2
3
4
5
6
7
8
9
10
SSW1
see Printer Manual
Epson
HP
9600
8
1
none
HWs
HP
9600
8
1
none
HWs
A:
A4 Paper
B:
1
2
3
4
5
6
7
8
1
2
3
4
5
6
7
8
see Printer Manual
13
2 Installation
2.4 Connecting the electrodes and sensors
On its rear panel the pH Meter pH960 has connections for a potentiometric
electrode 5, a separate reference electrode 6 and a temperature sensor 8.
Connect your electrodes and sensors according to the following diagram to
the switched off pH Meter:
5 Connection for potentiometric electrodes
pH, ISE, redox or silver electrodes with built-in or separate reference electrode; plug F
6 Connection for separate reference electrode
plug B, 4 mm
8 Connection for temperature sensor
Pt1000 or NTC, connected via two 2 mm banana plugs. Please
observe color classification for shielding purposes.
14
2 Installation
2.5 Mains connection
The pH Meter has an external power supply (PN3900-106) providing 12V
(DC). This is connected to 12V mains connection 12.
Mains cable
One of the following cables is supplied with the instrument
• PN 3900-107 Mains cable 2 Pol (C7) – EU (XVI)
• PN 3900-108 Mains cable 2 Pol (C7) – US (N1/15)
• PN 3900-109 Mains cable 2 Pol (C7) – GB (BS89/3)
• PN 3900-110 Mains cable 2 Pol (C7) – AUS (SAA/2)
and is connected to the external power supply.
Please make sure that the power supply is always kept dry. Protect it
against direct liquid contact .
2.6 Switch on
ON/OFF
After the selected accessories have been connected switch on the pH Meter
with the <ON/OFF> key (see also Sect. 4.3). The instrument will start in the
last operating mode to have been used for measuring pH, temperature or potential.
During the switch-on process an instrument checking routine is carried out
automatically. If an error message is displayed here ('Err x') then please
contact your local Precisa agency.
15
2 Installation
2.7 Initial configuration
The pH Meter is delivered with standard settings for the configuration and
method parameters. Many of these can be reset at any time by pressing the
<CLEAR> key during input (see also Sect. 4.3). If it should ever be necessary to reset the configuration of the instrument to its original condition then
this can be carried out by a re-initialization of the instrument memory (see
Sect. 8.5).
Before you start to make measurements please check the following configuration settings and, if necessary, alter them according to your own requirements. If you first want to make yourself familiar with the operation of the pH
Meter and the various editing possibilities then please read Sections 4.1, 4.2
and 4.4. More detailed explanations of the individual configuration settings
are given in Section 5.
Dialog language: english
CONFIG/Verschiedenes/Dialog:english
After this choice has been confirmed with <ENTER> the dialog language
changes immediately. For example, this item would then appear.
CONFIG/auxiliaries/dialog:english
Please switch the instrument off and on if this setting has been changed.
Date and time
CONFIG/auxiliaries/date
and /time
Please check that the date and time are correct.
Temperature sensor and unit
CONFIG/auxiliaries/Temp.sensor
and /Temp.unit
Enter the type of temperature sensor that is connected. If no temperature
sensor is connected and you always want to enter the measuring temperature
manually then you can ignore this setting.
16
3 Short operating tutorial
3 Short operating tutorial
In this section the necessary steps for carrying out a simple pH measurement
with calibration are described. The instructions are limited to those steps that
are absolutely necessary and will enable you to carry out your first measurements with the pH Meter directly. The operating principles are described in
Sect. 4.4.
3.1 pH measurement
3.1.1 Requirements
The following instruments, accessories and solutions are required for carrying
out the pH calibration and measurement described below:
• pH Meter pH960 (PN3900-096)
• 101 Magnetic Stirrer (PN 3900-103)
• pH electrode (enclosed)
with Pt1000 temperature sensor (e.g.: PN 3900-100 Unitrode)
• Calibration buffers
Precisa buffer solutions pH 4.00 (PN 3900-045) and
pH 7.00 (PN 3900-046)
3.1.2 Preparations
Before you start this short tutorial you must ensure that the instrument and
accessories have been correctly installed as described in Section 2. The most
important points concerning the installation are briefly given again below
(please refer to the Section mentioned for details). If you are not certain
whether all the settings (CONFIG and PARAMETER pH) correspond to the original conditions you can first reset any alterations by initializing the memory
(RAM Initialization) (see Sect. 8.5).
The calibration parameters for the pH mode are set for a calibration using two
Precisa buffers as default (see Sect. 6.2.2). If you want to use other buffers
then the corresponding buffer type must be entered.
17
3 Short operating tutorial
1
ON/OFF
2
CONFIG
pH Meter installation
• Set up instrument
• Connect stirrer
• Connect electrode
• Mains connection
Sect. 2.1
Sect. 2.2.1
Sect. 2.4
Sect. 2.5
Initial configuration
• Switch on pH Meter
• Set dialog language
• Set date/time
• Set temperature sensor
Sect. 5.4
Sect. 5.4
Sect. 5.4
Sect. 5.4
3.1.3 pH calibration
1
Start calibration with first buffer
• Immerse pH electrode in buffer solution pH 7
• Switch on stirrer with <STIRRER>
• Start calibration with <CAL>
• If no temperature sensor is connected:
enter the temperature and exit with <ENTER>
2
Continue calibration with second buffer
• Remove pH electrode from first buffer, rinse with water and
blot off gently with a lint-free tissue
• Immerse pH electrode in second buffer solution pH 4 and
continue calibration sequence with <ENTER>
3
Result
• Wait for potential measurement, result will be displayed:
CAL
ENTER
ENTER
18
• After 30 s the pH Meter will switch back automatically to the
measurement display. This can also be done immediately with
<ENTER>.
3 Short operating tutorial
4
ENTER
MODE
CAL.DATA
Poor calibration data
• If the calibration data are outside the calibration parameters
defined as the limits (see Sect. 6.2.2) then a corresponding
message will be shown:
• You can still accept the calibration data with <ENTER>, or reject it with <MODE>.
4
7
Show calibration data
• You can now display the calibration data with <CAL.DATA>.
If you move the selection bar to the end of the list with <”>,
then in the line
Curve
< -> >
you can activate the calibration curve display with <->>.
REPORT
9
4
Print calibration report
• With <REPORT> you can now output a calibration report to a
printer or a PC.
• With <CAL.DATA> you can jump directly to the short calibration report in the report selection list (calib short); this contains
all the data except the calibration curve itself.
• The Select key <->> offers the further option 'calib full';
this also outputs the calibration curve.
19
3 Short operating tutorial
3.1.4 pH measurement
1
CONFIG
Select printout criterion
• If the obtained measured value is to be printed out directly as
a measuring point report or transferred to a PC then the required printout criterion must be set
(see Sect. 5.2):
CONFIG/print meas.value/print crit.: drift
STIRRER
2
2
Start measurement
• Immerse the pH electrode in the sample.
• Switch on stirrer with <STIRRER>.
MEAS/
PRINT
3
Determine measured value
• You can read off the actual pH of the sample from the display.
It is stable when the drift display
(small double arrow on the left-hand side) no longer blinks.
4
Print measurement
• With <MEAS/PRINT> you can start the output of a measuring
point report on a printer or PC. The recording of the measurement and its output depend on the printout criterion 'Drift'
and take place only when the current drift condition is fulfilled
(see Sect. 6.2.1):
'mp
pH 960
02104 5.781.0012
date 2003-07-04 16:57:55
pH
********
run number
5
electr.id
#5
pH =
5.875
20.2 °C Pt1000
==============
20
4 Operation
4 Operation
4.1 The keypad
• Universal functions
• Input of numbers and text
• Navigation
• Special functions
The keys beneath the display can be triggered from the measured value display irrespective of the mode.
Most of the keys on the right-hand side have two functions: The numbers to
be entered and the navigation functions are shown in the center of the keys;
the additional functions at their upper margin.
21
4 Operation
4.2 Operating concept
The pH Meter provides two types of display:
1.
The measured value display.
This is the normal instrument display.
2.
The menu display
This is used for editing various settings.
In the directly measuring working modes the current measured value is
shown together with the date and time in the measured value display. If the
result is to be printed out, or if a stirring sequence or the entry of sample identifications (Id) are intended for recording a measured value, then this is
started with <MEAS/PRINT>. The measured value display changes when the
operating mode of the pH Meter is changed with <MODE>. You can easily
see which mode is set from the measuring unit or the prefix 'pH' shown in the
display.
In each operating mode you can switch from the measured value display to
the menu display with <CONFIG> or <PARAM>. This allows the instrument configuration and the method parameters to be edited. In the direct
measuring modes measurement recording and evaluation (e.g. automatic
printing and limit monitoring) continues in the background. In the menu display it is also possible to change directly from the configuration to parameter
input with <PARAM> and vice versa with <CONFIG>.
22
4 Operation
4.3 All key functions at a glance
The functions of all the keys are described below both for the measured value
display and the menu display:
Key
ON/OFF
Measured value display
(normal operation)
Menu display
(editing)
On/Off switch
On/Off switch
• The <ON/OFF> key switches the
instrument on and off
• The <ON/OFF> key switches the instrument off at any time.
• This applies even if the lamp of the
LCD display is switched off!
(see Sect. 5.4)
• After switch-on the pH Meter is in
the normal operation display of the
last mode to have been used
CONFIG
Opens configuration menu
Changes to configuration menu
• <CONFIG> opens the selection
menu for the instrument configuration.
• The <CONFIG> key can be used to
switch directly from the parameter menu
to the selection menu for instrument configuration.
• These configuration settings remain
unchanged until they are edited or
the permanent memory of the instrument configuration is initialized
(see Sect. 8.5).
Report selection
• Direct selection of the configuration
report after <REPORT>.
PARAM
Opens parameter menu
Changes to parameter menu
• The <PARAM> key opens the selection menu for the method parameters.
• With the <PARAM> key you can switch
directly from the configuration menu to
the parameter menu.
• All parameter settings belong to a
method and are stored methodspecifically with this method.
Report selection
• Direct selection of the configuration
report after <REPORT>.
Starts calibration
CAL
MEAS/
PRINT
• In the pH and mode the <CAL>
key starts a calibration.
Starts measurement / Prints
out measured value
• In the pH, T and U modes the
<MEAS/PRINT> key triggers a
23
4 Operation
Key
Measured value display
(normal operation)
Menu display
(editing)
measuring sequence.
• Depending on the configuration
(see Sect. 5.2), the <MEAS/PRINT>
key prints out the measured value
as a measuring point report.
MODE
QUIT
Operating mode selection
Cancels sequence
• In the pH, T and U modes the
<MODE> key changes the mode.
• With the <MODE> key working sequences are terminated without direct
transfer of the data.
Message acknowledgement
Cancels working step
• Displayed messages are normally
acknowledged with <QUIT>. (Exceptions: see Section 8.2)
• Queries are exited with <QUIT>. In this
way it possible, e.g. to skip individual
steps within a working sequence without
accepting the data.
• If cause of the message has not
been remedied then it will appear
again at the next check.
CAL.DATA
7
Displays calibration data
• In menus <QUIT> causes a jump to the
next higher level.
Enters the number '7'
• In the pH mode the <CAL.DATA>
key shows the current calibration
data.
Report selection
• Direct selection of the configuration
report after <REPORT>.
USER
8
REPORT
9
User selection
Enters the number '8'
• With <USER> a user name can be
newly entered, selected or deleted.
Report selection and printout
Enters the number '9'
• With <REPORT> a report can be
selected and printed out.
• The selection of the report from
those available is made either with
<SELECT> or directly by pressing
the corresponding key (e.g.
<CAL.DATA>, see right-hand column: Report selection).
Enters the number '4'
ADD.DATA
4
STORE
5
24
Stores measured value
• In the pH, T and U modes the
<STORE> key triggers a measuring
sequence and stores the measured
values in the memory in a similar
Enters the number '5'
4 Operation
Key
Measured value display
(normal operation)
Menu display
(editing)
manner to <MEAS/PRINT>.
• The storage criterion must have
been previously defined under
CONFIG /Store meas. value.
RECALL
6
Opens measured value
memory
Enters the number '6'
• The measured value memory is
opened with the <RECALL> key.
The stored measured values can
then be viewed or deleted.
Report selection
• Direct selection of the measured
value memory report after <REPORT>.
EL.TEST
1
Starts electrode test
Enters the number '1'
• In the pH mode you can start an
electrode test with the <EL.TEST>
key.
Report selection
• Direct selection of the pH electrode
test report after <REPORT>.
STIRRER
2
METHODS
3
Stirrer on/off
Enters the number '2'
• A connected stirrer can be switched
on and off manually with the
<STIRRER> key.
Method selection
Enters the number '3'
• With the <METHODS> key the selection for loading, saving or deleting a method is opened (see section
6.1).
Report selection
• Direct selection of the method
memory report after <REPORT>.
Enters the number '0'
0
ABC
.
Enters a decimal point '.'
• The <.> key enters a decimal point in
the input field.
Exception: open text editor
• If the <ABC> key is first pressed in an
input field where text input is possible
then a text input box for editing the text
25
4 Operation
Key
Measured value display
(normal operation)
Menu display
(editing)
will be opened.
Enters a minus sign '-'
-/exp
• If you start a numerical input with </exp> then the numerical value to be entered will receive a minus sign.
Enters an exponent 'E'
• When a numerical input has been started
then the <-/exp> key will provide an exponential notation.
SELECT
Selects predefined entries
and
• For menu parameters which offer a fixed
choice of settings (recognizable by the final colon) the selection list can be viewed
with the <SELECT>- keys. The arrows
determine the selection direction.
SELECT
Cursor control for text input
• In the text editor the arrow keys are used
to select the character to be entered and
the <ENTER> key to enter it.
CONTRAST+
and
CONTRAST -
Alters display contrast
Controls the menu bar
• The contrast of the LCD display can
be altered with the <CONTRAST+
> and <CONTRAST- > keys during
the measured values display.
• In each menu display the <“> and <”>
keys can be used to move the selection
bar up and down by one line.
• This setting is retained after the instrument has been switched off and
on. The default value is only reset after the memory has been initialized.
Cursor control for text input
• In the text editor the arrow keys are used
to select the character to be entered and
the <ENTER> key to enter it.
Leafing between entries in the
measured values memory
• Leafs between the entries in the measured values memory display: starting from
the last measured value to be stored you
can access older entries with <“> and
vice versa.
• At the beginning and end of the list you
can use the corresponding arrow key to
jump directly to the other end of the list.
Deletes text input
CLEAR
• Before opening the text editor during text
input the <CLEAR> key will delete the
complete entry. Within this box <CLEAR>
deletes the character to the left of the cursor.
Shows special value
26
• If a special value exists for an entry or se-
4 Operation
Key
Measured value display
(normal operation)
Menu display
(editing)
lection then this can be shown with
the<CLEAR> key.
Shows standard value
• All other entry and selection possibilities
provide the standard value with the
<CLEAR> key.
Confirms entry
ENTER
• The <ENTER> key is used to complete
each entry with the selection bar moving
on to the next parameter. If an entry is exited without this confirmation then the entered value will be rejected.
27
4 Operation
4.4 Operating principles
4.4.1 Configuration and method parameters
Instrument configuration and method parameters are each contained in
menus with a tree structure. These menu structures are shown in the Annex in
Section 9.3.
The instrument configuration of the pH Meter is described in the CONFIG
menu. This contains the basic settings that apply for all the selected working
modes and methods. The method parameters are stored under PARAMETERS. In contrast to the configuration, the method parameters depend on
the measuring mode which has been set.
The change from the measured value display to the menu display is made by
using the <CONFIG> or <PARAM> keys. The title of the submenu appears
first, and is shown with an '>' (e.g. >Measuring parameters). You can
now move the selection bar up and down with the <“> and <”> arrow keys.
Each underlying level in the menu structure is opened with <ENTER> and
exited with <QUIT>. Alterations to individual entries must be confirmed with
<ENTER>. If such alterations are exited with <QUIT> then they remain ineffective.
If an entry is confirmed with <ENTER> then the selection bar will move to the
next entry. At the end of a submenu it will finally change to the next point of
the superior menu selection.
In this way you can run through the complete menu structure for the configuration and parameters by repeatedly pressing the <ENTER> key. This can
be helpful when carrying out checks.
Not all parts of the menu structure described below are visible in the display
at all times. Only the specific possible settings of the option which is currently
activated are shown. For example, the various settings for printing out the
measured values under CONFIG/print meas. values/print crit. are
not visible when printing has been deactivated completely (OFF). If one of the
other printing criteria is selected then the particular settings it requires will appear in the display.
28
4 Operation
4.4.2 Editing menu entries
A basic differentiation is made between two types of menu entry.
SELECT
SELECT
Entries with a fixed selection are indicated by a colon:
dialog: english, deutsch, français, español
The selection is then made with the <SELECT> keys and confirmed with
<ENTER>. The default setting, which is normally shown in bold print, can be
shown by pressing <CLEAR>.
ENTER
Entries which can be edited are altered by entering a new value and confirming it with <ENTER>.
Numbers
are entered directly with the number keys. Exponential notation can be activated directly with the <-/exp> key.
Values outside the valid range of limits for the particular entry
will not be accepted by the instrument. This is indicated by
the invalid entry blinking. You can now either enter a new
value or retain the original value by exiting with <QUIT>.
Special entries exist for some numerical entries; these cannot
be seen directly and cannot be edited (e.g. 'OFF' for the
measuring parameter Drift). These can be shown with
<CLEAR> and confirmed with <ENTER>.
Text entries
are made using the text editor and are described in the
following section.
29
4 Operation
4.4.3 Entering text
ABC
.
You can use <ABC> to open a text editor for entering texts; this allows the
input of alphanumeric characters:
This text editor must be called up right at the start of a new entry after the old
entry has been completely deleted with <CLEAR>, if necessary. If a text input is started directly with numbers from the number block of the keyboard
then the subsequent opening of the text editor is no longer possible.
The required characters are selected with the arrow keys. The cursor movement can be accelerated by keeping the arrow keys pressed down. The
marked character is accepted in the input field with <ENTER>. A requirement is that a blinking cursor in the input field indicates that there free places
are available. Otherwise you can delete individual characters from the back
with <CLEAR>.
Text input is terminated by exiting the text editor with <QUIT> and confirming
the entry with <ENTER>. However, if the whole entry is to be rejected then
<QUIT> must be activated a second time.
30
5 Configuration
5 Configuration
CONFIG
With the <CONFIG> key you can access the configuration menu. This contains all the instrument settings for the pH Meter. These are independent of
both the mode and the method. This means that they cannot be stored separately like the method parameters (see Sect. 6). They continue to exist until
they are edited or the permanent memory containing the instrument configuration is re-initialized (see Sect. 8.5).
All the settings of this menu are described in this section. English is used as
the dialog language. For each point you will find all the possible entries or the
valid entry range together with the default value. This will always be reset
when the permanent memory of the pH Meter is re-initialized. During the input
you can also deliberately call up the default value with <CLEAR>. It is shown
in bold type below.
Example:
time interval
1,2,3...365...9999 d
This setting defines a time interval in days. In this example it is the time after
which the validation of the instrument is to be carried out (>monitoring/validation). You can either enter whole numbers between 1 and 9999
or call up the default value of 365 days with <CLEAR>.
31
5 Configuration
5.1 Report
REPORT
9
CONFIG
+ report
¦ + id1
: + id2
+ report id
+ instrument id
+ date & time
+ method
+ electrode id
+ signature
+ line feed
In the configuration menu report you can define the output format of the report header. This describes the first lines of a measuring point report (see
also Sect. 7.2.3) and can be either placed in front of each measured value to
be printed out or before a series of measured values (see following section).
A report header containing all the elements described here could look like
this:
Report Id:
Instrument Id:
Date, Time:
User*:
Mode / Method / Run number:
Electrode Id:
Sample Id1:
Sample Id2:
'mp
pH960
date 2003-07-05 09:50:56
user
pH
pH-1
electr.id
id1
batch 21
id2
sample A01
Signature: Signature
5.781.0012
C. Weber
run number
9
pH electr.1
________________________
*The 'user' line is not configured here. The entry of a user name takes place
automatically when a user has been defined with the <USER> key. The
name remains active until it is deleted or another user name is selected (see
Sect. 4.3).
id1, id2
(max. 16 characters)
This is where you can define short texts as additional information for the report header. Each of these entries will be printed out in a single line in each
report. In addition, you can also request these Ids before each measurement
as a preselection (see method parameter preselections in Sect. 6), e.g. in
order to mark each sample specifically.
report id:
ON, OFF
This setting defines whether the report Id is to be printed out in the first line of
the report header. It is used to identify the report.
instrument id:
32
ON, OFF
5 Configuration
You can include the instrument identification in the report header if you want
to. It consists of the exact type name of the pH Meter with the version number
of the instrument software.
An additional way of assigning report printouts to a particular instrument is by
using an individual instrument name under CONFIG/auxiliaries/device
label (see Sect. 5.4). This will then be printed out automatically in a separate
line in the report header after the instrument Id.
date & time:
ON, OFF
This setting defines whether the date and time of the report printout are to be
printed. The date and the exact time of the measurement can additionally be
printed with each successive measured value (see following section).
method:
ON, OFF
As well as the mode name, the name of the method used can also be printed
out in the report header if required. You can define this previously by storing
the method parameters used with <METHODS>. If no method name has yet
been defined then the character sequence ******** will appear.
electrode id:
ON, OFF
You can include the electrode name in the report header if you have defined
an electrode ID for the currently valid calibration. Otherwise this field in the report header will remain empty.
signature:
ON, OFF
Reports which contain measuring data (measuring point, calibration and electrode test reports) can, depending on the configuration, have a signature line
added on. In this way the result can be provided with a signature.
line feed
form, 0,1,2,3...999
The paper feed of the printer at the end of a report can be set here. With continuous paper printers (e.g. Custom) you can select the number of empty
lines so that after the report has been printed out you can tear off the printed
paper directly at a suitable point. For single page printers (e.g. HP DeskJet)
you can enter the special value 'form' with <CLEAR> so that the printed
page will automatically be produced by the printer after each report.
33
5 Configuration
5.2 Printing out measured values
MEAS/
PRINT
CONFIG
:
+ print meas.value
: + print crit ¦
¦
+
¦
¦
¦
¦
+
¦
¦
+
¦
¦
¦
+
immediate
time
drift
plot
+
+
+
+
+
+
+
+
+
+
+
date & time
report header
calibration report
date & time
report header
calibration report
time interval
stop time
date & time
report header
calibration report
time interval
time scale
time scale label
stop time
OFF
In the configuration menu print meas.values the output form of measured
values, triggered by <MEAS/PRINT>, is defined. This is only possible for the
direct measuring modes pH, T and U.
print crit:
immediate, time, drift, plot, OFF
Depending upon the print criterion a measured value report with be transmitted via the RS 232 interface to a printer or PC either immediately, at defined
time intervals or only when a drift condition has been fulfilled. If a stirring sequence is intended before the measurement (PARAMETERS/measuring parameters/stirrer: control, see Sect. 6), then these print criteria will
only be effective when the stirring sequence has been concluded.
A further way of documenting the measured values is to output a graphical
plot of the measure value signals.
print crit.:
immediate
With this setting a measured value report will be produced when
<MEAS/PRINT> is activated from the normal instrument display. The following options can be used:
date & time:
ON, OFF
Here you can choose whether the date and time at which the measured
value was recorded are to be included with each individual measured
value. This can take place irrespective of whether a report header is
used.
report header:
34
once, always, OFF
5 Configuration
Normally each measured value is accompanied by the report header
for documentation purposes. The exact contents of the report header
are defined under CONFIG/Report (see above).
With a larger series of manually triggered measurements it may be advisable to print out the report header only once with the first measured
value. In this case all the measurements should be made under the
same conditions. The report header will only appear again when the run
number has been reset to zero by switching the instrument off and on.
calibration report:
ON, OFF
You have the possibility of providing each measured value with the associated calibration data of the electrode used, e.g. within the context
of a GLP documentation.
print crit:
time
With this print criterion you can automatically record and output the measured
values at fixed intervals. The following options are used:
date & time:
report header:
calibration report:
ON, OFF
once, always, OFF
ON, OFF
These settings correspond to those of the print criterion 'immediate'
(see above).
time interval:
0.1...4.0...99999.2 s
Automatic measuring value recording can be carried out at time intervals of down to 0.1 s. Please note that if small time intervals are used
then the amount of data for each measured value must be adapted accordingly, as otherwise the buffer memory of the connected printer or
PC would be filled too quickly. This means, for example, that the report
header should only be printed out once at the start of a series of measurements. Otherwise data could be lost at the RS232 interface of the
receiver. In this case you should consider matching the measured value
recording interval to the measured value memory (see Sect. 5.3).
stop time:
OFF, 1...999999 s
The time after which an automatic series of measurements is to be terminated can be entered in whole seconds. You can also let a series of
measurements run indefinitely without a fixed stop time and then stop it
manually with <QUIT> if you select 'OFF' for this setting.
35
5 Configuration
print crit.:
drift
If this print criterion is used then a measured value will only be documented
when the drift condition defined under PARAMETERS/measuring parameters/drift has been fulfilled.
date & time:
report header:
calibration report:
ON, OFF
once, always, OFF
ON, OFF
These settings correspond to those of the print criterion 'immediate'
(see above).
print crit.:
plot
The directly recorded values can be outputted graphically as a measured
value/ time plot.
time interval:
0.1...4...99999.2 s
In a similar way to the print criterion 'time' a time interval can be defined for graphical measured value recording.
time scale:
5,10,30,60,120,180..99960 s/cm
This is the time axis scale. The reciprocal value of the quantity entered
corresponds to the paper feed rate. This means that, e.g., for a required
feed rate of 2 cm/min a time scale of ½ min/cm = 30 s/cm must be entered.
time scale label.: rel, abs
The time axis scale can use the relative time in minutes and seconds
(start = 0 s). The current time can also be used with 'abs'.
stop time:
OFF, 1...999999 s
The graphical plot is terminated when the stop time has elapsed or will
continue indefinitely ('OFF'). In both cases termination is possible with
<QUIT>.
36
5 Configuration
5.3 Storing measured values
STORE
5
CONFIG
:
+ store meas. value
: + store crit
+
immediate, drift, OFF
time - time interval
+ stop time
In the direct measuring modes pH, T and U you can use <STORE> to store
up to 100 measured values with additional information in the instrument
memory (see Sect. 7.3). The functions of the settings to be defined under
CONFIG/store meas. value correspond to those made under CONFIG/print meas. value:
store crit:
immediate, time, drift, OFF
This storage criterion also only becomes effective when an optional stirring
sequence has been concluded.
In contrast to the report output, the combination of the information stored together with each measured value is fixed.
store crit:
immediate
The current measured value is stored with <STORE>.
store crit:
time
time interval:
stop time:
0.1...4.0...99999.0 s
OFF, 1...999999 s
You can automatically record and save the measured values at fixed time intervals until the stop time has been reached.
store crit:
drift
A measured value can also be stored when the drift condition defined under
PARAMETERS/measuring parameters/drift has been fulfilled.
After 100 measured values have been stored, and each time a further storage
attempt is made, the pH Meter will produce a corresponding warning:
measured value memory full
You now have the possibility of using <RECALL> to view the stored measured values, of deleting individual measured values or of clearing the whole
measured value memory (see Sect. 7.3). It is also possible to output all
measured values as a report via the RS232 interface (see Sect. 7.2.7).
5.4 Auxiliaries
37
5 Configuration
CONFIG
:
+ auxiliaries
: + run number
+ last digit
+ dialog
+ display
+ LCD off after
+ date
+ time
+ time zone
+ temp.sensor
+ temp.unit
+ device label
+ beep
+ program
Various basic settings for the configuration of the pH Meter are made in this
submenu.
run number
0,1,2,3...999, OFF
The run number is included in the report. It is increased by one after each
measuring process. This applies to both the storage of measured values and
to the calibration or pH electrode test and makes the later chronological assignment of such different measuring processes easier.
When the instrument is switched on the run number is automatically set to '0'.
The first measuring process begins with '1'.
last digit:
ON, OFF
This setting can be used to conceal the last decimal place of the measured
value display. The displayed value is rounded off accordingly. This can be
useful in improving the readability of a rapidly changing measured value.
Please note that this setting does not influence the drift control of a measurement.
dialog:
english, deutsch, français, español
The dialog language covers both the language shown on the display and that
used in the report. Switch the instrument off and on if this setting has been
changed.
display:
positiv, negativ
You can choose whether you want to have a positive or negative display
presentation, e.g. in order to adapt it to the local lighting conditions.
LCD off after
1,2...999 min, OFF
The display of the pH Meter has an illuminated background. In order to increase the working life of the lamp you can switch off the display automatically when the instrument has not been used for a certain time. Please note
38
5 Configuration
that, if the lamp is switched off and on too frequently then its working life will
also be reduced. This means that times of about 30 min can be recommended.
The fact that the LCD illumination is switched off does not affect the functioning of the pH Meter in any way. It continues to work normally. The lamp can
be activated again with any key except <ON/OFF>. Please note that the
<ON/OFF> key switches the instrument off. All other keys only have the
function of activating the LCD illumination. This means, for example, that runs
will not be terminated when the <QUIT> key is used to reactivate the background illumination.
date
time
YYYY-MM-DD
hh:mm:ss
You can set the date and time here. The program will only accept numbers
which make sense.
time zone
12 ASCII characters
For complete documentation you can add details of the time zone to the time
information for output in the report header. The input of up to any 12 characters is possible. Examples: 'MEZ', 'UTC-05:00' (Coordinated Universal
Time minus 5 h) or location of the measurement.
temp.sensor:
Pt1000, NTC
The pH960 pH Meter supports the use of two different types of temperature
measuring techniques T: Pt1000 (platinum resistance thermometer) and NTC
('Negative Temperature Coefficient' semiconductor). This means that the configuration must be adapted accordingly. If NTC sensors are used then it is
also necessary to enter two sensor characteristics; these can be found in the
specification of the sensor:
R(25 °C)
B value
10000...30000...100000
1000...4100...9999
39
5 Configuration
temp.unit:
C, F
The pH Meter can work with temperature information in both °C and °F units.
Please note that, when changing this setting, the default value of the measuring parameter drift in the T mode has the unit °C and, if necessary, must be
converted as follows:
TF = 32 + 1.8 ·TC
or
TC = (TF – 32)/1.8
TF: temperature in °F
TC: temperature in °C
device label
12 ASCII characters
If apart from the instrument Id you wish to assign a further name to a particular pH Meter for inclusion in the report then you can enter your text here, e.g.
'Lab 2.01' or 'Works 2'. This will then be included in the report header in a
separate line inserted after the instrument Id.
beep:
OFF,1,2,3
Messages on the display of the pH Meter are accompanied by a beep. This
can be switched off completely or just limited to a sequence of 2 or 3 beeps.
program
This is the version number of the instrument software and cannot be altered. It
is included in the report header as part of the instrument Id.
40
5 Configuration
5.5 Monitoring
CONFIG
:
+ monitoring
: + validation
+ service
+ system test
report
The pH960 pH Meter can inform you automatically about reoccurring quality
monitoring tasks.
validation: ON, OFF
time interval
time counter
1...365...9999 d
0 d
If this option is active then you can enter a time interval in days and, when it
has elapsed, the instrument will request you to carry out a validation process.
In addition, the time counter shows the elapsed time in days since the last
time that this option was switched on. When the time counter reaches the set
number of days then the following message will appear:
validate instrument
This will also be included in the report header. It can only be removed in the
following ways:
•
Resetting the time counter to zero under CONFIG/monitoring/ validation with <CLEAR>
•
Extending the time interval and then switching the instrument off and on
again
•
Switching off the validation monitoring option
In order to prevent unauthorized removal of the message the <CONFIG> key
can be disabled under the instrument SETUP (see Sect. 7.5.1), so that the
settings described above are no longer accessible.
service:
next service
ON, OFF
YYYY-MM-DD
At a particular time the instrument can remind you about the date when a service is due. When the set date has been reached the following message appears on the display:
service is due
This is also included in the report header and can be switched off by either
entering a new and later service date or by switching this monitoring function
off.
41
5 Configuration
system test report:
ON, OFF
When it is switched on the pH960 pH Meter automatically carries out a system diagnosis. The result can be outputted as a system test report (see Sect.
8.4.1).
5.6 Peripheral units
CONFIG
:
+ peripheral units
: + character set
+ dosimat
+ stirrer
+ keyboard
+ barcode
Various peripheral units can be connected to the pH960 pH Meter. The corresponding configurations must be carried out here.
character set:
IBM, Epson, Seiko, Citizen, HP
The type of printer chosen for the report printout is selected here. If you have
connected a PC to the RS 232 interface for data reception then set this parameter to 'IBM'.
stirrer:
101
The stirrer 101 can be switched on and off from the pH Meter with <STIRRER>. The stirring rate can also be controlled from the pH Meter (see PARAMETERS/measuring parameters/Stirrer).
keyboard:
US, deutsch, français, español,
schweiz.
If texts have to be entered frequently it may be a good idea to connect a PC
keyboard. The language-specific keyboard layout is then set here. Older PC
keyboards may possibly have a too-high power consumption, which could
result in the cancellation of the system test when the instrument is switched
on. In such a case remove the connected keyboard and switch on the instrument again.
42
5 Configuration
barcode:
input, id1, id2
For data input you can also use a barcode reader which provides a PS/2
connection. Older barcode reader may possibly have a too-high power consumption, which could result in the cancellation of the system test when the
instrument is switched on. In such a case remove the connected keyboard
and switch on the instrument again.
5.7 RS 232 settings
CONFIG
:
+ RS232 settings
+ baud rate
+ data bit
+ stop bit
+ parity
+ handshake
For communication with instruments (printer, PC) connected to the serial
RS232 interface the correct setting of these parameters is required:
baud rate:
data bit:
stop bit:
parity:
handshake:
38400, 19200, 9600, 4800, 2400, 1200,
600, 300
7, 8
1, 2
even, none, odd
HWs, SWChar, SWline, none
Please refer to the manual of your printer for the exact settings. When a computer is connected the corresponding configuration can usually be carried out
in the terminal program used.
43
6 Methods / Parameters
6 Methods / Parameters
The exact measuring method of the pH Meter is described by method parameters which, like the instrument configuration, are arranged in a tree structure in the menu display. The complete tree is shown in the Annex (Sect. 9.3)
to provide a better overview.
The parameters are set in a similar way to the instrument configuration. In
contrast, however, the administration of the method parameters is modespecific. The selection of the method parameters also varies with the selected
mode. For this reason the method parameters for each mode are described
separately in this section.
This means that one of the following subsections, together with the instrument
configuration, forms a complete description of all the settings which are important for the operation of the pH Meter in a particular measuring mode.
6.1 Method management
METHODS
3
Press <METHODS> if you want to save all current parameter settings as a
method. You can also load or delete methods within this dialog.
METHODS
+ recall method
+ store method
+ delete method
For each selection you can edit a method name with <ABC> or select one
with <SELECT>.
All saved methods are accessible in all modes. If you load a method which
requires a different mode than the actual, the pH Meter will switch to this
mode automatically.
44
6 Methods / Parameters
6.2 pH measurement (pH mode)
6.2.1 Measuring parameters
PARAMETER pH
¦
+ measuring parameters
: + electr.id
+ drift pH
+ temperature*
+ method
+ delta measurement
+ stirrer
(* only appears if no temperature sensor is connected)
The measuring parameters describe the settings which are of direct importance for the measurement.
electr.id:
12 ASCII characters
You can assign any name you like to the connected pH electrode. During a
calibration the resulting calibration data will be assigned to this entered electrode Id and stored. The electrode Id will then be included in the report
header for the output of measured values.
In this way you can enter several electrode Ids. This allows you to switch between various pH electrodes with their associated calibration data. However,
a requirement is that each new electrode Id is linked with a new calibration.
Then you can use <SELECT> under the measuring parameter Electr.Id to
select one of the stored electrode Ids.
In order to delete an electrode Id and its linked calibration data this must be
reset under <CAL.DATA> (Reset cal., see Sect. 7.1.1).
drift pH
0.005...0.050...9.999/min, OFF
A measuring signal which changes as a function of time is regarded as being
sufficiently constant when its drift drops below the value defined here. This
can be used as criterion for the pH Meter if a displayed measured value is to
be stored or documented by printing a report (see print criterion and storage
criterion in Sect. 5.2 and 5.3). Please note that for a drift-controlled measured
value recording this drift parameter must not be set to 'OFF', as otherwise no
result will be exported.
If the drift condition is not fulfilled then this is indicated by two constantly
blinking triangles in the display.
An active drift control increases the reproducibility of the measurements as a
constant condition is used to define the measured result. A smaller value for
the measuring parameter Drift pH requires a more stable measuring signal
than a larger one. The set measuring parameter is also proportional to the
measuring uncertainty of the measured value obtained.
45
6 Methods / Parameters
Please note that the drift condition defined here and the temperature parameter described below do not apply to the calibration and, if necessary, must be
set separately under the calibration parameters.
temperature
-999.9...25.0...999.9 °C
This menu item only appears when no temperature sensor is connected. In
this case you can enter the temperature of the sample solution here. If the
measuring and calibration temperatures are different then it is necessary to
record the temperature for the automatic correction of the electrode slope
(temperature compensation, see Sect. 9.2.1). Information about the measuring temperature is also absolutely necessary for the complete documentation
of a pH value. In the report printout of the measured value this manually determined temperature is indicated by the suffix 'manual'.
method
8 ASCII characters
All parameter settings can be stored together or loaded as a method (see
Sect. 6.1). The name of the current method is then given here. This field is
only used for information here and cannot be edited directly.
delta measurement
ON, OFF
:The delta measurement permits the display of the measured value relative to
a freely selectable constant reference value:
reference pH
-19.999...0.000...19.999
This reference value is subtracted from the measured value itself. The modified measured value is shown together with this value and is taken into consideration, for example, in checking the limit values (see PARAMETER
pH/limits pH). The reference value is not included in the report. However,
should you still want to document it then you should also produce a parameter report (see Sect. 7.2.6).
stirrer:
ON, OFF, control
You can choose whether the pH measurement is to be made while stirring is
being carried out or not. A requirement is that a stirrer is connected with a
suitable cable. If the 101 stirrer has been connected and the settings made
under CONFIG/peripheral units then the stirring rate can also be selected:
stirring rate
1...5...15
If you want your measurement to be made without stirring but still want to stir
the solution before the measurement then you should select the control setting. In this way you can trigger a stirring sequence before the start of each
measurement with <MEAS/PRINT>:
prestir pause
stir time
poststir pause
46
0...99999 s
0...99999 s
0...99999 s
6 Methods / Parameters
The prestir and poststir pauses represent waiting periods in which stirring
does not take place. The measurement itself only starts when the complete
stirring sequence has ended.
Please note that this parameter is binding for the report output and for storing
a measured value. Therefore when you start a measurement with <MEAS
/PRINT> the stirrer will be switched on and off accordingly. This is why you
should preferably carry out drift-controlled measurements (see Sect. 5.2
and Sect. 5.3).
6.2.2 Calibration parameters
PARAMETER pH
:
+ calibration parameters
: + temperature*
+ Drift
+ report
+ calibration interval
+ no.of buffers
+ buffer type
+ low lim.slope
+ up lim.slope
+ low lim.pH(0)
+ up lim.pH(0)
+ offset Uoff state
(*only appears if no temperature sensor is connected)
The calibration parameters describe the most important settings for the calibration such as buffer types and tolerance values. The evaluation of the pH
calibration is described in Sect. 9.2.1.
temperature
0.0...25.0...99.9 °C
Just as for the measuring temperature, the calibration temperature should
also be entered when no temperature sensor is connected. If the measuring
and calibration temperatures are different then this is absolutely necessary for
the automatic temperature correction of the electrode slope. The temperature
is also stored with the suffix 'manual' and marked in this way in the calibration report.
The exact temperature recording is also important for the pH calibration as
the pH Meter works with automatic buffer recognition (see below: buffer
type).
47
6 Methods / Parameters
drift
0.1...0.5...9.9 mV/min
Just as in the pH measurement, the potential measurement for the pH calibration is drift-controlled. However, this drift control cannot be switched off.
Please note that, in contrast to pH measurement, the drift for the pH calibration is entered in mV/min. It is therefore inevitably different from the drift for pH
measurement (see Sect. 6.2.1).
Report:
OFF, short, full
After the calibration it is possible to output the calibration data automatically
in the form of a report. You should chose between the 'short' version which
contains all the relevant data and the 'full' version which additionally shows
the calibration curves in the form of a graph (see Sect. 7.2.4).
Such a report can also be exported at a later date with the calibration data of
each stored electrode Id.
calibration interval OFF, 1...999 h
The pH Meter can automatically remind you about any recalibration of the pH
electrode which is due. This means that if a calibration is carried out with a
preset calibration interval then, when this interval has elapsed, a message will
appear on the display:
cal.interval expired
This message remains and will be printed out on every measuring point report until a new calibration has been carried out.
number of buffers
1, 2...9
Up to 9 buffers can be used for the pH calibration. If calibration is carried out
with only one buffer then the program will use the theoretical value of 100.0%
for the slope. This also applies when a calibration with several buffers is canceled with <MODE> or <QUIT> after the first buffer has been measured
and then confirmed with <ENTER>.
If three or more buffers are used then the variance will be included in the calibration data. More detailed information about the evaluation is given in Sect.
9.2.
48
6 Methods / Parameters
buffer type:
Precisa, Metrohm, NIST, DIN, Fisher,
Fluka-BS, Mettler, Merck, Beckman,
Radiometer, special, own, mixed
For the automatic temperature-specific buffer recognition during the calibration and for the electrode test, information about the type of buffer used is required. In the pH Meter the temperature-dependent pH values of reference
buffer solutions and technical buffer solutions from some suppliers are
stored. Such a buffer table for Precisa buffers looks like this:
Precisa buffers
T [°C]
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
pH 4.00 pH 7.00 pH 9.00
3.99
3.99
3.99
3.99
3.99
4.00
4.00
4.01
4.02
4.03
4.04
4.06
4.07
4.09
4.11
4.13
4.15
4.18
4.20
4.23
7.11
7.08
7.06
7.04
7.02
7.00
6.99
6.98
6.98
6.97
6.97
6.97
6.97
6.98
6.98
6.99
7.00
7.00
7.01
7.02
9.27
9.18
9.13
9.08
9.04
9.00
8.96
8.93
8.90
8.87
8.84
8.81
8.79
8.76
8.74
8.73
8.71
8.70
8.68
8.67
The other stored buffer tables are described in Sect. 9.4. During the calibration the pH Meter shows the type and temperature-specific pH value of the
recognized buffer. For temperatures within the 5 °C steps the pH value is
linearly interpolated.
buffer type:
special
If you would like to use different buffers from those described, then you
require the exact pH value of each buffer at the temperature used for
calibration. These pH values can be entered here. During the calibration
they can again be adapted before each measurement.
buffer type:
own
If further temperature-specific pH values are known for such buffers
then under own you can enter up to five such pH(T) series at steps of 5
49
6 Methods / Parameters
°C. The query starts at 0 °C and finishes at 95 °C or earlier, if 'OFF' is entered with <CLEAR>.
If you do not know the pH values for individual temperatures just enter
zero. However, you can also calculate these values by linear interpolation and enter them. Missing pH definitions will otherwise be shown during the calibration by negative values; the calibration will then be interbuffer not defined.
rupted with the error message
buffer type:
mixed
A further way of using the stored buffer table is to combine a maximum
of five different buffer types to form a new series. You can make your
selection from all the stored buffers described in Sect. 9.4. It is possible
to select buffers from those defined under Buffer type: own.
A general rule is that you can only calibrate in defined temperature ranges, as
otherwise the error message:
buffer not defined
appears. If you use more than two buffers for the calibration then you can use
certain buffers several times in order to give them a better statistical weight.
low lim.slope
up lim.slope
low lim.pH(0
up lim.pH(0)
0.1...95.00...999.9 %
0.0...103.0...999.9 %
-99.999...6.40...99.999
-99.999...8.00...99.999
)The most important calibration data such as slope and pH(0) must lie within
the limits defined here in order for them to be automatically adopted. The
given default values for the slope correspond to the quality criteria of a "passing electrode" in the electrode test (see Sect. 8.7).
If one of the values of the calibration data lies outside these limits then at the
end of the calibration the following message will appear: cal. data out of
limits; you can then accept or reject the results.
offset Uoff state: OFF, ON
offset Uoff
-2200.0...0.0...2200.0 mV
The automatic buffer recognition of the pH Meter assumes an offset potential of 0 ± 30 mV for the electrode used. Ag/AgCl reference electrodes normally meet this requirement. If other reference systems are
used, e.g. a calomel electrode, then the offset potential may be outside
this range. This means that for correct buffer recognition this variation
must be compensated by entering the specific offset potential Uoff. For
the pH measurement itself this parameter is unimportant.
6.2.3 Limits pH
PARAMETER pH
50
:
+ limits pH
: + state
6 Methods / Parameters
In the direct measuring modes the pH Meter has a limits function which allows the control of the parameter to be monitored. The control signals are
transmitted via the MSB. Out of limits conditions are also shown on the display and documented in the report.
state:
u.limit
u.hyst.
l.limit
l.hyst.
ON, OFF
pH
pH
pH
pH
-19.999...14.000...19.999
-19.999...0.020...19.999
-19.999...0.000...19.999
-19.999...0.020...19.999
The exact way in which the limits function works is described in Section 7.4
independent of the mode.
6.2.4 Limits T
PARAMETER pH
:
+ limits T
: + state
As well as the primary measuring quantity pH, the temperature can also be
controlled by the limits function. However, you should only activate the limits
function for the temperature when a temperature sensor is connected, as
otherwise an error message will appear.
state:
ON, OFF
u.limit
u.hyst.
l.limit
l.hyst.
-999.9...100.0...999.9 °C
-999.9...0.2...999.9 °C
-999.9...0.0...999.9 °C
-999.9...0.2...999.9 °C
The exact way in which the limits function works is described in Section 7.4
independent of the mode.
6.2.5 Plot parameters
PARAMETER pH
:
+ plot parameters
: + left mar. pH
+ right mar. pH
+ left marg.T
+ right marg.T
51
6 Methods / Parameters
The two directly recorded measuring quantities pH and temperature can be
printed out as a function of time in a plot. Under CONFIG/print meas.
value the print criterion 'plot' must be selected (see Sect. 5.2). The scales
of the measured values axes are determined by the following limits.
left mar. pH
right mar. pH
left marg.T
right marg.T
TIP !
-19.9...0.0...19.9
-19.9...14.0...19.9
-999...20...999 °C
-999...30...999 °C
The value for the right-hand limit of a plot must not necessarily be the larger
one. By exchanging the limits the plot of the particular quantity can be mirrored.
6.2.6 Preselections
PARAMETER pH
:
+ preselections
+ req.ident
req.ident.:
id1, id1 & id2, OFF
For sample identification you can document each measured value with two
Ids in the report header. These can either be predefined under CONFIG/report and included in each report or, depending on the
Preselections setting, they can be requested before each measurement.
Please note that sample identifications requested as a preselection before the
measurement will also be stored as an entry under CONFIG/report. This
means that they are again available for the next measurement.
52
6 Methods / Parameters
6.2.7 Electrode test
PARAMETER pH
:
+ electrode test
: + electrode type
+ temperature
+ report
The pH Meter can carry out a pH electrode test, which permits the quality of
the electrode used to be evaluated. A detailed description of the electrode
test is given in Sect. 8.7.
electrode type: standard, gel, non-aq., own
Various types of pH electrodes have different evaluation criteria. For the three
most commonly used Metrohm pH electrode types the tolerances are stored
in the pH Meter: standard electrodes, gel electrodes and non-aqueous electrodes.
electrode type: own
If you wish to define your own tolerances then select 'own'. You can
now enter the limits for the quality features 'excellent electrode',
'good electrode' and 'passing electrode'. An explanation of the
individual limits is given in Sect. 8.7.3.
Regardless of the electrode evaluation, if 'own' is selected as the electrode type then you can also edit the limits for the offset potential Uoff.
This allows the electrode test to be carried out with pH electrodes
which, even with an Ag/AgCl reference electrode, show a clearly shifted
zero potential (e.g. antimony electrode). The use of other reference
electrodes can also result in changed zero potentials.
temperature
0.0...25.0...99.9 °C
If no temperature sensor is connected then enter the temperature at which
the buffer will be measured here.
report:
OFF, short, full, line
After the electrode test you can automatically output the result in the form of
report. You can choose between the 'short' version containing all the relevant
data and the 'full' version, which also shows the measuring curves as a graph.
If you are only interested in the evaluation of the electrode itself then select
'line'. Only the result will be printed out, e.g. 'excellent electrode'. If no
printer is connected then please select 'OFF'.
The report of the last pH electrode test can also be printed out later with
<REPORT> (see Sect. 4.3).
53
6 Methods / Parameters
6.3 Temperature measurement (T mode)
6.3.1 Measuring parameters
PARAMETER T
+ measuring parameters
: + electr.id
+ drift
+ method
+ delta measurement
+ stirrer
The measuring parameters describe the settings of direct importance for the
measurement.
electr.id
12 ASCII characters
You can assign any name you want to the connected temperature sensor.
This sensor Id is then contained in the report header for measured values.
drift
0.5...1.0...999.9 °C/min, OFF
A measuring signal which changes as a function of time is regarded as being
sufficiently constant when its drift drops below the value defined here. This
can be used as criterion for the pH Meter if a displayed measured value is to
be stored or documented by printing a report (see print criterion and storage
criterion in Sect. 5.2 and 5.3). Please note that for a drift-controlled measured
value recording this drift parameter must not be set to 'OFF', as otherwise no
result will be exported.
If this drift condition is not fulfilled then this is indicated by two constantly
blinking triangles in the display.
An active drift control increases the reproducibility of the measurements as a
constant condition is used to define the measured result. A smaller value for
the measuring parameter Drift requires a more stable measuring signal than a
larger one. The set measuring parameter is also proportional to the measuring uncertainty of the measured value obtained.
method
8 ASCII characters
All parameter settings can be stored together or loaded as a method (see
Sect. 6.1). The name of the current method is then given here. This field is
only used for information here and cannot be edited directly.
delta measurement:
ON, OFF
The delta measurement permits the display of the measured value relative to
a freely selectable constant reference value:
reference
-999.9...0.0...999.9 °C
This reference value is subtracted from the measured value itself. The modified measured value is shown together with this value and is taken into consideration, for example, in checking the limit values (see PARAMETER
54
6 Methods / Parameters
T/limits T). The reference value is not included in the report. However,
should you still want to document it then you should also produce a parameter report (see Sect. 7.2.6).
stirrer:
ON, OFF, control
You can choose whether the pH measurement is to be made while stirring is
being carried out or not. A requirement is that a stirrer is connected with a
suitable cable. If the stirrer 101 has been connected and the settings made
under CONFIG/peripheral units then the stirring rate can also be selected:
stirring rate
1...5...15
If you want your measurement to be made without stirring but still want to stir
the solution before the measurement then you should select the control setting. In this way you can trigger a stirring sequence before the start of each
measurement with <MEAS/PRINT>:
prestir pause
stir time
poststir pause
0...99999 s
0...99999 s
0...99999 s
The prestir and poststir pauses represent waiting periods in which stirring
does not take place. The measurement itself only starts when the complete
stirring sequence has ended. Please note that this parameter is binding for
the report output and for storing a measured value. Therefore when you start
a measurement with <MEAS/PRINT> the stirrer will be switched on and off
accordingly. This is why you should preferably carry out drift-controlled
measurements (see Sect. 5.2 and Sect. 5.3).
6.3.2 Limits T
PARAMETER T
+ limits T
: + state
In the direct measuring modes the pH Meter has a limits function which allows the control of the parameter to be monitored. The control signals are
transmitted via the MSB. Out of limits conditions are also shown on the display and documented in the report.
state:
u.limit
u.hyst.
l.limit
l.hyst.
ON, OFF
-999.9...100.0...999.9 °C
-999.9...0.2...999.9 °C
-999.9...0.0...999.9 °C
-999.9...0.2...999.9 °C
The exact way in which the limits function works is described in Section 7.4
independent of the mode.
You should only activate this limits function for the temperature if a temperature sensor is connected, as otherwise the following message will appear
limit error
55
6 Methods / Parameters
6.3.3 Plot parameters
PARAMETER T
+ plot parameters
: + left mar.
+ right mar.
The measured temperature can be printed out as a function of time in a plot.
Under CONFIG/print meas. value the print criterion 'plot' must be selected (see Sect. 5.2). The scales of the measured values axes are determined by the following limits.
left mar.
right mar.
TIP !
-999.9...0.0...999.9 °C
-999.9...100.0...999.9 °C
The value for the right-hand limit of a plot must not necessarily be the larger
one. By exchanging the limits the plot of the particular quantity can be mirrored.
6.3.4 Preselections
PARAMETER T
+ preselections
+ req.ident
req.ident:
id1, id1 & id2, OFF
For sample identification you can document each measured value with two
Ids in the report header. These can either be predefined under CONFIG/report and included in each report or, depending on the Preselections
setting, they can be requested before each measurement.
Please note that sample identifications requested as a preselection before the
measurement will also be stored as an entry under CONFIG/report. This
means that they are again available for the next measurement.
56
6 Methods / Parameters
6.4 Potential measurement (U mode)
6.4.1 Measuring parameters
PARAMETER U
¦
+ measuring parameters
: + electr.id
+ drift
+ method
+ delta measurement
+ stirrer
The measuring parameters describe the settings which are of direct importance for the measurement.
electr.id
12 ASCII characters
You can assign any name you like to the connected pH electrode. The electrode Id will then be included in the report header for the output of measured
values.
drift
0.5...1.0...999.9 mV/min, OFF
A measuring signal which changes as a function of time is regarded as being
sufficiently constant when its drift drops below the value defined here. This
can be used as criterion for the pH Meter if a displayed measured value is to
be stored or documented by printing a report (see print criterion and storage
criterion in Sect. 5.2 and 5.3). Please note that for a drift-controlled measured
value recording this drift parameter must not be set to 'OFF', as otherwise no
result will be exported.
If this drift condition is not fulfilled then this is indicated by two constantly
blinking triangles in the display.
An active drift control increases the reproducibility of the measurements as a
constant condition is used to define the measured result. A smaller value for
the measuring parameter Drift requires a more stable measuring signal than a
larger one. The set measuring parameter is also proportional to the measuring uncertainty of the measured value obtained.
method
8 ASCII characters
All parameter settings can be stored together or loaded as a method (see
Sect. 6.1). The name of the current method is then given here. This field is
only used for information here and cannot be altered directly.
57
6 Methods / Parameters
delta measurement:
ON, OFF
The delta measurement permits the display of the measured value relative to
a freely selectable constant reference value:
reference
-2200.0...0.0... 2200.0 mV
This reference value is subtracted from the measured value itself. The modified measured value is shown together with this value and is taken into consideration, for example, in checking the limit values (see PARAMETER
U/limits U). The reference value is not included in the report. However,
should you still want to document it then you should also produce a parameter report (see Sect. 7.2.6).
stirrer:
ON, OFF, control
You can choose whether the pH measurement is to be made while stirring is
being carried out or not. A requirement is that a stirrer is connected with a
suitable cable. If the stirrer 101 has been connected and the settings made
under CONFIG/Peripheral units then the stirring rate can also be selected:
stirring rate
1...5...15
If you want your measurement to be made without stirring but still want to stir
the solution before the measurement then you should select the control setting. In this way you can trigger a stirring sequence before the start of each
measurement with <MEAS/PRINT>:
prestir pause
stir time
poststir pause
0...99999 s
0...99999 s
0...99999 s
The prestir and poststir pauses represent waiting periods in which stirring
does not take place. The measurement itself only starts when the complete
stirring sequence has ended. Please note that this parameter is binding for
the report output and for storing a measured value. Therefore when you start
a measurement with <MEAS/PRINT> the stirrer will be switched on and off
accordingly. This is why you should preferably carry out drift-controlled
measurements (see Sect. 5.2 and 5.3).
6.4.2 Limits U
PARAMETER U
+ limits U
: + state
In the direct measuring modes the pH Meter has a limits function which allows the control of the parameter to be monitored. The control signals are
transmitted via the MSB connection. Out of limits conditions are also shown
on the display and documented in the report.
state:
58
ON, OFF
6 Methods / Parameters
u.limit
u.hyst.
l.limit
l.hyst.
-2200.0...1000.0...2200.0 mV
-2200.0...2.0...2200.0 mV
-2200.0...-1000.0...2200.0 mV
-2200.0...2.0...2200.0 mV
The exact way in which the limits function works is described in Section 7.4
independent of the mode.
6.4.3 Plot parameters
PARAMETER U
:
+ plot parameters
: + left mar.
+ right mar.
The measured potential can be printed out as a function of time in a plot. Under CONFIG/print meas.value the print criterion 'plot' must be selected
(see Sect. 5.2). The scales of the measured values axes are determined by
the following limits.
Left mar.
Right mar.
TIP !
-2200.0...-1000.0...2200.0 mV
-2200.0...1000.0...2200.0 mV
The value for the right-hand limit of a plot must not necessarily be the larger
one. By exchanging the limits the plot of the particular quantity can be mirrored.
6.4.4 Preselections
PARAMETER U
:
+ preselections
+ req.ident
req.ident:
id1, id1 & id2, OFF
For sample identification you can document each measured value with two
Ids in the report header. These can either be predefined under CONFIG/report and included in each report or, depending on the Preselection
setting, they can be requested before each measurement.
Please note that sample identifications requested as a preselection before the
measurement will also be stored as an entry under CONFIG/report. This
means that they are again available for the next measurement.
59
7 Various functions
7 Various functions
This section describes various functions of the pH Meter which cannot be assigned to individual modes.
7.1 Calibration data
The current pH calibration data can be called up at any time with the
<CAL.DATA> key.
A detailed description of the evaluation of the calibration measurements for
the calculation of this data can be found in Sect. 9.2.
An overview appears which, depending on the measuring mode and calibration data, can have a different composition.
For example, if no calibration has yet been carried out for a new electrode Id
then only the theoretical calibration data slope = 100.00% and pH(0) = 7.000
will be shown and taken into account for the measurement.
60
7 Various functions
7.1.1 pH calibration data
CAL.DATA
7
CAL.DATA
+ electr.id
+ method
+ slope
+ pH(0)
+ temperature
+ temp.sensor
+ c.dat.
+ cal.interval
+ variance
+ buffer type
+ no.of buffers
+ cal.table:
+ b1
+ b2
:
+ bn
+ curve
electr.id
If an electrode Id has been selected or entered under PARAMETER pH/
measuring parameters/electr.id before the calibration then it will be
shown here. The calibration data apply only to this electrode and will change
when a new electrode Id is set under the above measuring parameters (see
Sect. 6.2.2).
method
The calibration parameters set under PARAMETER pH/calibration parameters form part of the method parameters. The corresponding method
name will be shown here if the calibration data has been obtained with this
method and the resulting quantities slope and pH(0) have not been altered
since. If no method name has been issued before the calibration (see Sect.
6.1) then '********' will appear here.
slope
The slope of the linear calibration curve obtained during the calibration will be
shown here as a percentage. This is a relative quantity which is based on the
temperature-specific value of the Nernst constant (e.g. 59.16 mV at 25 °C).
Without a calibration, or after a single buffer calibration, this is set to 100%.
This value can be altered manually for test purposes. However, afterwards the
information about the method will be missing from the list and from the calibration data report. The calibration date and time will be updated and the
temperature information and the calibration table (see below) will be removed. In addition this action will be documented by the entry 'manual' under
CAL.DATA/variance.
pH(0)
61
7 Various functions
This is the second characteristic quantity of the calibration curve. pH(0) is the
pH value at 0 mV. It can also be altered manually for test purposes. The other
entries under CAL.DATA will be altered in the same way as for a manual alteration of the slope (see above).
temperature
The calibration temperature is shown here.
temp.sensor
If the calibration temperature has been determined automatically by a connected temperature sensor then its type will be shown here ('Pt1000' or 'NTC').
A manually entered temperature for the calibration will be indicated accordingly ('manual').
c.dat.
The date and time of the calibration is shown here.
cal.interval
If a calibration interval has been defined under PARAMETERS pH/ calibration parameters/cal.interval then it will be shown here. It can be used
together with the calibration time given under c.dat. to estimate the time that
the next calibration is due.
variance
If at least 3 calibration buffers have been used then the calibration function
will be calculated as a compensation curve according to the principle of the
smallest mean-square error (linear regression). The resulting variance will be
given here. A more detailed explanation of these calculations is given in Sect.
9.2.1.
Each subsequent manual alteration of the calibration data pH(0) and slope
will be documented by the entry 'manual' against these parameters.
buffer type
The type of buffer defined in the calibration parameters at the time when calibration was carried out is shown here.
62
7 Various functions
no.of buffers
The number of buffers actually measured is shown here. This can be lower
than that given in the calibration parameters, as a calibration can be terminated prematurely with <QUIT>; only the buffers which have already been
measured will then be used for the calculation of the calibration data.
cal.table:
original, delete n, reset cal
This entry can be used to delete individual buffers from the calibration table
('delete n') or to delete all the calibration data of an electrode Id ('reset
cal').
original
If you use <SELECT> to chose the option 'original' then all the buffer
data previously deleted with 'delete n' will be reinserted in the calibration table and used for calculating the calibration data.
delete n
From a calibration list containing at least 3 buffer entries you can remove individual buffer data by selecting 'delete n' and entering the
number of the buffer to be deleted in the following line:
delete n:
1..9
The deleted buffer will then be indicated in the calibration table by 'deleted'. The measuring points of deleted buffers are also indicated in
the graphical display by an 'o' instead of a '+'.
You can reinsert all deleted buffers in the calibration table with the option 'original'.
reset cal
With this option you can reject all the calibration data of an electrode Id.
They are then in the same state as before the first calibration (slope =
100%, pH(0) = 7).
Although the electrode Id is retained, it cannot be selected under PARAMETER pH/measuring parameters/electr.id until it has been
calibrated again.
63
7 Various functions
b1, b2...bn
For each calibration buffer the pH value used and the measured potential are
given. The given value for the pH is taken from the stored series of buffers of
the buffer type selected in the calibration parameters (see Sect. 9.4). The pH
values for temperatures within the given 5 °C steps are calculated by linear interpolation.
A buffer which has been deleted by cal.table: delete n is shown here by
'deleted'.
curve
< –> >
If at least 2 calibration buffers have been used then the calibration curve will
be shown as a graph here. The graphics display is accessed with <’>:
This display is exited with <QUIT>.
64
7 Various functions
7.2 Reports
A pH Meter report is produced by transmitting data to a printer or PC via the
RS232 interface. In this way you can document e.g. measuring results, calibration data, method parameters or the configuration of the instrument in written form.
A requirement for a properly functioning report output is the input of the receiving instrument (see Sect. 5.6) and the correct setting of the RS232 transmission parameters (see Sect. 5.7).
The following reports can be automatically printed out after a measurement
has been made: a measuring point report is produced directly with the
<MEAS/PRINT> key. The automatic output of calibration, electrode test
and result reports must be defined as such under method parameters.
REPORT
9
Apart from the measuring point report, all reports can be triggered manually
at a later date by the <REPORT> key. A dialog appears for the selection of
the required report with the <SELECT> keys:
user memory
Report of the memory occupancy by methods and calibration data
calib short
Calibration report without graphical calibration function
curve
calib full
Calibration report with graphical calibration function
curve
config
Instrument configuration report
param
Current method parameters report
el.test
pH electrode test report (see Sect. 8.7)
mv memory
Output of all stored measured values
all
Output of all existing reports
During selection these reports can also be selected directly by using the key
which has the corresponding function (e.g. <CAL.DATA> for a calibration
report).
65
7 Various functions
The following table shows the availability of all reports in the various modes
together with the direct selection keys.
pH
T
U
Direct key
user memory
P
P
P
-
calib short
P
-
-
<CAL.DATA>
calib full
P
-
-
-
config
P
P
P
<CONFIG>
param
P
P
P
<PARAM>
el.test
P
-
-
<EL.TEST>
mv memory
P
P
P
<RECALL>
all
P
P
P
-
The report output can be terminated at any time with <QUIT> or
<MODE>. For this reason you should wait for the report output to be
finished before operating the pH Meter again. In this way you avoid
the accidental cancellation of a report output.
The following pages show the arrangement of reports together with some
types of reports. A description of an electrode test report is given in Sect. 8.7.
66
7 Various functions
7.2.1 Arrangement of a report
The first lines of a report provide a general description. This report header is
configured under CONFIG/Report (see Sect.5.1):
Report Id:
Instrument Id:
Date, Time:
'mp
pH 960
02104 5.781.0012
date 2003-07-08 17:00:56
...
For the output of data as measuring points, results, calibration or electrode
test reports further information about the mode, method, sample number and
electrode Id is included:
Report Id:
Instrument Id:
Date / Time:
User:
Mode / Method / Run number:
Electrode Id:
'mp
pH 960
02104 5.781.01012
date 2003-07-08 17:00:56
user
C. Weber
pH
pH-1
run number
9
electr.id
pH electr.1
...
Signature:
signature ______________________________
Depending on the configuration, in such measuring data reports a signature
line can be added to the data.
The line 'user' appears, if a user is defined by <USER>.
If you have entered an instrument name under CONFIG/auxiliaries/ device label then this will appear in the report header as an additional line
between the Instrument Id and the Date/Time line.
In measuring point and result reports the report header contains additional information about the measured sample as Id 1 and Id 2, if these have been
defined under CONFIG/report or are requested before the measurement as
a preselection (see PARAMETER/preselections).
Each report is concluded with a finishing line. For an automatically triggered
original report (measuring points, results, calibration or electrode test reports) this is in the form of a double line:
==============
Each report to be triggered manually with <REPORT> is concluded with a
single line:
--------------
67
7 Various functions
7.2.2 Report identification
The report identification, known here as Report Id, is an abbreviation describing the type of report and is primarily important for the remote control of the
pH Meter via the RS232 interface.
The following report Ids exist for the pH960 pH Meter:
Report Id
Report name
measuring points
configuration
parameter
user methods
measured values stored
pH calibration report
full pH calibration
diagnose
electrode test
'mp
'co
'pa
'um
'mv
'cr
'fp
'di
'et
7.2.3 Measuring point report
MEAS/
PRINT
By pressing the <MEAS/PRINT> key in the directly measuring measurement
types a measuring point report will be produced. The following examples
show versions of this type of report, the various configurations of which are
defined under CONFIG/print meas.value (see Sect. 5.2).
A typical version of a measuring point report is the output of a single measured value. The print criterion 'immediate' or 'Drift' must be selected.
'mp
pH 960
02104 5.781.0012
date 2003-07-08 17:00:56
user
C. Weber
pH
pH-1
run number
9
elektr.id
id1
charge 21
id2
sample A01
#1
pH =
8.182
21.2 °C (Pt1000)
2003-07-08 17:00:56
==============
68
7 Various functions
If a whole series of measured values is to be documented then this is done
by selecting under CONFIG/Print meas. values the option Report
header: once. In this way the report header will be printed out once with
the first measured value. Each further time that the <MEAS/PRINT> key is
pressed a further measured value will be printed out:
#2
#3
#4
#5
pH =
8.185
2003-07-08
pH =
8.187
2003-07-08
pH =
8.188
2003-07-08
pH =
8.189
2003-07-08
21.2 °C
17:01:56
21.2 °C
17:02:56
21.2 °C
17:03:56
21.2 °C
17:04:56
(Pt1000)
(Pt1000)
(Pt1000)
(Pt1000)
Such a series of measured values can also be produced automatically by selecting the print criterion 'time'.
With the print criterion 'plot' the measured values are given out as a graphical plot in the direct measurement types. As well as configuration under CONFIG/print meas.value, the scales of the measured values curves must be
set under PARAMETER/plot parameters (see plot parameters in Sect.
6.2 ). In the pH mode the measured temperature can also be shown in the
same plot as a secondary measured value in addition to the primary measured value, pH:
'mp
pH960
date 2003-07-08
user
pH
pH-1
elektr.id
02104
17:00:56
5.781.0012
C. Weber
run number
9
pH electr.01
Temperature scale
pH scale
Temperature curve
pH curve
L. limit pH
U. limit pH
==============
69
7 Various functions
7.2.4 Calibration report
REPORT
9
CAL.DATA
+
7
In the pH modes a calibration report can be produced after a calibration has
been carried out. Under PARAMETER/calibration parameters/report
you can define whether this report is to be produced automatically after the
measurement. You can also choose between a short version containing all
the important data and a long version which additionally contains a plot of the
calibration function.
'fp
pH 960
02104 5.781.0012
date 2003-07-08 17:10:16
user
C. Weber
pH
pH-1
run number
9
elektr.id
pH electr.01
pH calibration
temperature
20.1 °C
temp.sensor
Pt1000
c.dat.
2002-07-08 17:06
buffer type
Precisa
buffer 1
buffer 2
buffer 3
variance
slope
pH(0)
pH
7.019
3.991
9.037
U/mV
0.1
176.7
-115.4
1.192
99.44 %
7.035
==============
7.2.5 Configuration report
A configuration report (CONFIG) could look like this:
REPORT
70
9
+
CONFIG
dpH
-0.015
0.006
0.009
7 Various functions
'co
pH 960
02104 5.781.0012
date 2002-07-09 10:03:55
CONFIG
>report
id1
id2
report id:
ON
instrument id:
ON
date & time:
ON
method:
ON
electrode id:
ON
signature:
OFF
line feed
3
>print meas.value
print crit:
immediate
date & time:
OFF
report header:
always
calibration report:
OFF
>store meas.value
store crit:
OFF
>auxiliaries
run number
3
last digit:
ON
dialog:
english
display:
positiv
LCD off after
OFF min
date
2003-07-09
time
10:03:55
time zone
temp.sensor:
Pt1000
temp.unit:
C
device label
beep:
1
program
5.781.0012
>monitoring
validation:
OFF
service:
OFF
system test report:
OFF
>peripheral units
character set:
IBM
Dosimat:
765
stirrer:
101
keyboard:
US
barcode:
input
>RS232 settings
baud rate:
9600
data bit:
8
stop bit:
1
parity:
none
handshake:
HWs
--------------
71
7 Various functions
The settings shown for the instrument configuration correspond to the standard settings in the normal operating condition of the pH Meter after the configuration memory has been initialized (see Sect. 8.5) followed by conversion
to English as the dialog language.
7.2.6 Parameter report
REPORT
9
+
PARAM
in order to document the parameter settings for the current method you can
produce a parameter report:
'pa
pH 960
02104 5.781.0012
date 2003-07-09 12:08:36
PARAMETER pH
>measuring parameters
electr.id
drift
0.050 /min
method
********
delta measurement:
OFF
stirrer:
OFF
>calibration parameters
drift
0.5 mV/min
report:
OFF
cal.interval
OFF h
no.of buffers
2
buffer type:
Precisa
low lim.slope
95.00 %
up lim.slope
103.0 %
low lim.pH(0)
6.40
up lim.pH(0)
8.00
offset Uoff state:
OFF
>limits pH
state:
OFF
>limits T
state:
OFF
>plot parameters
left mar.:
0.0
right mar.:
14.0
left marg.T
20 °C
right marg.T
30 °C
>preselections
req.ident:
OFF
>electrode test
electrode type:
standard
report:
OFF
--------------
The standard parameters following a memory initialization in the current mode
are shown; in this case the pH mode with a connected temperature sensor
(see Sect. 8.5). Such parameters can be stored as a method (see Sect. 6.1).
72
7 Various functions
7.2.7 Measured values memory report
REPORT
9
RECALL
+
6
In the direct types of measurement you can store up to 100 measured values
with <STORE> (see Sect. 7.3). If you want to print out all the stored data
then you can produce a measured values stored report:
'mw
pH 960
date 2003-07-09
02104
13:55:20
5.781.0012
#1
pH
7.254
temp. (Pt1000)
20.1 °C
Id1
smpl. 1-1
date 2003-07-09 13:54:10
method
pH Demo
#2
pH
6.923
temp. (Pt1000)
20.1 °C
Id1
smpl. 1-2
date 2003-07-09 13:54:22
method
pH Demo
#3
pH
6.575
temp. (Pt1000)
20.1 °C
Id1
smpl. 1-3
date 2003-07-09 13:54:36
method
pH Demo
--------------
The entries for Id1, Id2, User and Method will only be included in the report if
they contain data.
Please note that this is a simple and rapid method of producing measured
values with their most important data. For the complete documentation of
measured value results in the sense of the normal quality assurance requirements you should select the automatic measuring point report instead.
73
7 Various functions
7.2.8 User method report
METHODS
REPORT
9
+
3
Method and calibration data occupy memory space in the pH Meter. The user
method report gives an overview of the memory occupancy:
'um
pH 960
02104 5.781.0012
date 2003-07-09 13:58:49
user memory
>methods
pH
pH-Demo
82
Conc F(-1)
F-Determ
64
>caldata
pH
pH 1.1
130
Conc F(-1)
F-Sens
146
remaining bytes
4578
--------------
The mode, method name and the occupied memory is given in bytes for each
of the methods. For calibration data the mode, electrode Id and memory occupancy are given.
A total of 5000 bytes is available for this data. This means that you can store a
maximum of approx. 50 methods or calibration data. This number can vary
depending on the size of the individual data records.
The size of the measured value memory (see Sect. 7.3) is independent of this
memory administration.
74
7 Various functions
7.3 Measured values memory
In the direct measuring modes pH, T and U the pH Meter can store up to 100
measured values with additional information. Depending on the storage criterion you can store the measured values immediately, at fixed time intervals
or drift-controlled.
The appropriate instrument settings are made under CONFIG/Store meas.
value and their functions correspond to the settings for printing the measured values. A more detailed description of the configuration is given in Sect.
5.3.
7.3.1 Save measured values
Saving measured values is triggered with <STORE>. Each storage process
is indicated with a beep and a message, e.g.:
STORE
5
measured value
31 stored
After 100 measure values have been stored, and after each further attempt to
store a measured value, the pH Meter will produce a warning message:
measured value memory full
You now have the possibility of using <RECALL> to view the stored data or
of deleting individual measured values or the whole measured values memory
(see Sect. 7.3.3).
7.3.2 Print measured values
REPORT
9
RECALL
+
6
The output of all stored measured values to a printer or computer via the
RS232 interface is made as a measured values memory report (see Sect.
7.2.7). This is done by pressing <REPORT> when in the measured values
display and then selecting the measured values stored report directly with
<RECALL>.
75
7 Various functions
7.3.3 Show measured values
RECALL
6
With <RECALL> the menu for displaying or deleting stored measured values
is called up:
measured value memory
>show measured values
del mv store:
no
Select the item Show measured values in order to access the corresponding display. The last measured value to have been stored with the highest
number will always be shown first:
Measured value no. No. of stored MVs
CONTRAST+
CONTRAST -
You can now use the two arrow keys <“> and <”> to leaf between the
measured values. With <“> you can access older entries and with <”>
newer ones. You can also leaf beyond the first and last entries and can in this
way access the first entry from the last one and vice versa.
By pressing <CLEAR> the displayed entry in the measured value memory will
CLEAR
be deleted directly. In this way you can select any measured value in the list
and delete it individually. The numbering of the other entries will be
changed accordingly, i.e. all the following measured values will receive a
lower number.
In order to delete all measured values you should use <SELECT> in the
above measured values memory menu to select the second choice del mv
store: and set it to 'yes'; then confirm this and the following safety query
delete ? with <ENTER>.
76
7 Various functions
7.4 Limit monitoring
In all the direct measuring modes pH, T and U it is possible to monitor the
current measured value with respect to certain upper and lower limits. In the
mode pH the temperature can also be monitored.
Under PARAMETERS/limits you can activate limits monitoring. Depending
on the measuring mode you may be able to monitor the limits of a secondary
measured value in addition to the primary measured value. You can define
the upper and lower limits and the particular hysteresis. A detailed description
of the parameter settings in each measuring mode is given in Section 6.2.
If a limit is exceeded then a beep will be heard and the following message will
appear on the display:
limit error
This message cannot be removed with <QUIT>. It will vanish automatically
as soon as the measured value again lies within the defined limits when the
hysteresis is taken into account.
7.4.1 Uses
Documentation
If 'time' or 'plot' has been selected as a print criterion under CONFIG/print meas.value then the displayed measured value will be transferred via the RS232 interface to a printer either as a measuring point report
or as a plot. In the measuring point report each measured value which lies
limit error.
outside the defined limits will be indicated by the message
In the plot the limits are clearly shown as a dotted line. An example of a printout can be found in Section 7.2.3.
77
7 Various functions
7.4.2 How it functions
The exact way in which limit monitoring functions and the effect on the remote
outputs are shown in the following diagram.
measured
value
u. limit
u. hysteresis
l. hysteresis
l. limit
signal output
time
aktive
u. limit
inaktive
aktive
l. limit
inaktive
Fig. 7:
Remote outputs in limit monitoring.
The lower and upper limits and the associated hysteresis are the characteristic quantities for limit monitoring. They can be defined in the parameter settings for each measuring mode (see Sect. 6.2 to Fehler! Verweisquelle konnte
nicht gefunden werden.). The lower or upper limit is always the triggering
point for the activation of the corresponding remote line or for the message
on the display. If the upper limit is again undercut or the lower limit exceeded
again then the activation will continue until the so-called hysteresis range has
also been exited. This avoids the too frequent activation or deactivation of the
alarm function when the measured value oscillates very closely around a limit.
This means that the activation cancellation point is defined as the upper limit
minus hysteresis and the lower limit plus hysteresis.
Set the hysteresis to zero, if you are just interested in an exact documentation
of limit overruns.
78
7 Various functions
7.5 Setup
Certain settings of the pH Meter can be found in the Setup menu. This menu
cannot be accessed from the normal instrument display, as alterations to
these settings have a great influence on the functions of the pH Meter.
The Setup menu is called up immediately after the instrument has been
switched on by pressing down and holding down the <CONFIG> key.
setup
+ lock
+ input assign
+ graphics
+ instr.number
Be very careful when making alterations in this menu! Alterations have
a very large influence on the functions of the instrument. Accidental alterations can be rejected by carrying out a deliberate memory initialization (see Section 8.5).
7.5.1 Locking
setup
+ lock
: + all keys
+ <CONFIG>
+ <PARAM>
+ <CAL>
+ recall method
+ store method
+ delete method
+ <CAL.DATA>
+ <MODE>
+ <EL.TEST>
You can disable certain keys and functions, e.g. to prevent unwanted alterations to the instrument settings or method parameters.
You can activate such a disablement by setting the corresponding parameter
to 'ON'. This does not affect access to the Setup menu in any way.
Please note that configuration settings (i.e. CONFIG/report/id1 and id2)
and parameters (i.e. manual calibration concentrations or standard additions), which are edited during a measurement or calibration procedure, are
modified that way even if <CONFIG> or <PARAM> are locked. The advantage is that the requested settings and parameters only have to be confirmed
during repeated procedures.
Please note that all disablements will be invalidated if a RAM-Init is carried out
(see Section 8.5).
79
7 Various functions
7.5.2 Input assignment
setup
:
+ input assign
: + Mode pH
+ Mode T
+ Mode U
+ Start pH cal.
+ Start el.test
+ <ENTER>
1
2
3
5
6
15
The assignment described here represents the default setting.
7.5.3 Graphics
setup
:
+ graphics
: + grid
+ frame
+ width
+ length
In order to provide the graphical plot of the report printout with a frame and a
grid you should switch on the corresponding options.
You can adapt the width and length of this plot to the size of the printer paper used by altering the particular factor (0.4 ... 1.0).
80
8 Troubleshooting – Messages – Maintenance
8 Troubleshooting – Messages –
Maintenance
8.1 Troubleshooting
If problems occur during pH or ISE measurement then these can have various causes:
1. Application
Difficult sample matrices or interferences can prevent reliable measurements.
2. Buffer / Standard solution
The precision of pH and ion measurements depends primarily on the correction calibration of the electrode. You should use clean and fresh buffer
solutions and standard solutions. For example, a frequent cause of incorrect calibration is the use of an old pH 9 or pH 10 buffer, whose pH can
vary considerably from the certified pH of a new buffer as a result of the
absorption of atmospheric CO2.
3. Measuring / Reference electrode
The electrodes are the most important element of the whole measuring
system. The correct handling of the measuring and reference electrodes is
described in the leaflet which accompanies the electrode.
4. pH Meter
If the pH Meter is thought to be the cause of a measuring problem then
first check all the configuration and parameter settings. The diagnostic
functions help you in searching for the fault (see Sect. 8.5). In addition,
you can also check the measuring input by using the Calibrated Reference (see Sect. 8.6).
The pH Meter will inform you directly about problems during the measurement. These messages are explained in the following Section 8.2. A further
possibility of carrying out a selective search for a pH electrode fault is the
electrode test. This is described in Sect. 8.7, where you will also find specific
measures for remedying any fault discovered during the test.
81
8 Troubleshooting – Messages – Maintenance
The following table lists general problems that can occur during pH and ISE
measurements. Possible causes and appropriate remedies are also described.
Symptom
Cause
Measuring signal absent Electrode not connected
or very variable
Air in or in front of the diaphragm
Faulty electrode
Measured value remains dirty pH or ISE membrane or diaphragm
unstable and does not
pH or temperature of the solution is not
fulfill drift criterion.
stable
Remedy
• Connect electrode
• Remove air
• Replace electrode
• Clean membrane or diaphragm
• Measure under exclusion of air
• Thermostat the solution
Unsuitable electrode:
• Conductivity too low
• Organic solution
• Use suitable electrode
Electrode not connected
• Connect electrode
Faulty electrode
• Replace electrode
Measured value reached dirty pH or ISE membrane or diaphragm
slowly
• Clean membrane or diaphragm
Slope too small on calibration
pH or ISE membrane or diaphragm is
dirty
• Clean membrane or diaphragm
Glass membrane dehydrated after
measurement in non-aqueous solution
• Immerse electrode in water between measurements
Poor buffer/standard solutions
• Replace buffers or standards
Electrode "used up"
• Replace electrode
Incorrect calibration
• Check and repeat calibration
• Check buffer/standard solutions,
replace if necessary
Manual temperature input incorrect
• Enter correct temperature of the
solution
dirty pH or ISE membrane or diaphragm
• Clean membrane or diaphragm
Electrolyte or electrode too old
• Refill electrolyte or replace electrode
Faulty electrode
• Replace electrode
With standard addition
'auto' the potential step
'delta U' is not reached.
Streaming potential of the measuring or
reference electrode causes potential difference between addition in stirred and
measurement in unstirred solution
•
•
•
•
System test message:
system error #X
Instrument fault
• Note error number and inform
Precisa Service
Measured value obviously incorrect
lower dosing rate
increase stirring rate
increase 'delta U'
'auto dos' instead of 'auto'
8.2 Messages
The pH Meter uses various messages to selectively inform you about possible errors or operating problems. These are shown in the bottom line of the
display and illustrated by a symbol in front:
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8 Troubleshooting – Messages – Maintenance
Type
Symbol
Example of a message
Error
same buffer
Warning
cal.data out of limits
Information
manual stop
change buffer <ENTER>
calibration OK
Monitoring
cal.interval expired
These messages can normally be removed by pressing the <QUIT> key.
However, some messages will remain until their cause has been remedied.
For example, this applies to a monitoring message.
Please note that you should not press <QUIT> to acknowledge a
message while a report is being produced as this will cancel the report.
The following table lists alphabetically all the messages which could appear
on the display of the pH Meter.
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8 Troubleshooting – Messages – Maintenance
Message
Situation
Cause
Remedy
XXX bytes
missing
Method storing
XXX bytes are missing for
saving a method
buffer alloc.
impossible?
pH calibration
• Buffer not recognized or 1. Replace buffer
not defined (buffer type 2. Press <ENTER>
'special', 'own' or 'mixed') 1. Stop calibration
Press <QUIT> to delete
old methods
or
2. Define buffer
3. Restart calibration
84
or
• Offset potential Uoff is
set too high
Enter Uoff (see Sect. 6.2.2)
and restart calibration
Enter missing value in temperature table (see Sect.
6.2.2)
buffer not
defined
pH calibration
pH of a buffers has not
been defined under
Buffer type: own for
the given temperature
buffers
unsuitable
Electrode test
Electrode test has been
started with a set of buffers
that does not contain all
the necessary buffers
calibration
interval expired
pH
Set calibration interval has
expired
Recalibrate electrode
(see Sect.)
calibration OK pH calibration,
Calibration has been concluded successfully
Exit display with <QUIT>;
this happens automatically
after 30 s; calibration data
will be accepted
cal.data out
of limits
pH calibration
Determined calibration
data are outside limits defined as calibration parameter
Accept calibration data with
<ENTER> or reject them
with <MODE>; check
electrode, buffer or limits
under 6.2.2
change buffer
<ENTER>
pH calibration
Instrument is waiting for
new buffer
1. Change buffer
check electrode
Temperature
measuring
Short circuit or interruption
Remedy fault or change
mode
• Change buffers
• Check selected buffer
type in the calibration parameters (see Sect.
8.7.1)
2. Press <ENTER>
8 Troubleshooting – Messages – Maintenance
Message
Situation
Cause
Remedy
----.- °C
or Various runs with
check T-sensor temperature
measurement
Temperature sensor is
faulty or has been unplugged during the run
delta T >2 °C
pH calibration
Temperature difference be- 1. Match temperatures
tween 2 buffers is too large 2. Continue with <ENTER> or cancel with
<MODE> and restart
Electrode test
Temperature difference be- 1. Cancel electrode test with
<MODE>
tween 2 buffers is too large
Connect a properly
functioning temperature
sensor
2. Restart with suitable buffers.
electrode test Electrode test
not passed
Electrode test gives values
outside the tolerances
limit error
Direct measurement, all modes
Set limit for primary or sec- see Sect. 7.4
ondary measured value
exceeded
manual stop
Various measuring runs
Measurement has been
stopped manually
measuring
Various measurrange exceeded ing runs
see Sect. 8.7.4
• Electrode not immersed Remedy fault or change
in the solution
mode
• Electrode not connected
correctly
measured value Saving measured
memory full
values in a direct
measurement
Attempt made to store a
further measured value
when 100 have already
been stored
Delete measured values
(see Sect. 7.3)
please wait
new task was started during report output
Wait for report output
Report output
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8 Troubleshooting – Messages – Maintenance
Message
RS232
remote control
RS receiver error:
parity unmatched
1. Press <QUIT>
RS232
remote control
RS receiver error:
stop bit unmatched
1. Press <QUIT>
RS232
remote control
RS receiver error:
data overflow, at least one
character cannot be read
(incorrect baud rate)
1. Press <QUIT>
RS232
remote control
RS receiver error:
internal receiver buffer
overflow
1. Press <QUIT>
Report output
RS transmitter error: handshake not replied to for at
least one second
1. Press <QUIT>
RS error 36
RS error 39
RS error 42
Remedy
Press <QUIT> and
Report output
RS error 38
Cause
Data output is faster than
printer processing speed
plot data
overflow
RS error 37
86
Situation
• Increase time interval between measurements
• Increase time scale
• Reduce graph width
• Only output primary
measured value.
2. Match the parities of both
instruments
(see Sect. 5.7)
2. Match the stop bits of
both instruments
(see Sect. 5.7)
2. Match the baud rates of
both instruments
(see Sect. 5.7)
2. Repeat process
2. Check reception readiness at other end
RS error 43
Report output
RS transmitter error:
transmission from the pH
Meter has been interrupted
by XOFF for at least three
seconds
• Press <QUIT>
• Send XON
RS error 45
Report output
RS transmitter error:
The receiver buffer of the
pH Meter contains an incomplete character string
(line feed missing); this has
blocked pH Meter transmission
• Press <QUIT>
• Send line feed
same buffer
pH calibration
Potential difference between 1st and 2nd buffer
< 6 mV
1. Change buffer
2. Press <ENTER>
8 Troubleshooting – Messages – Maintenance
Message
Situation
Cause
Remedy
service is due Instrument has
been switched on
Set service date has been
reached
stirrer not
found
An attempt has been made 1. Press <QUIT>
to control an 101 stirrer
2. Switch off instrument
which is not connected
3. Check stirrer connection
Various situations
Contact service
(see Sect. 5.5)
or
• Check measuring parameters
system error #X
1. Note error number
System test after
switch on
pH Meter fault
T mode
Temperature sensor is
faulty or not connected
Connect a properly functioning temperature sensor
transmission
error
PC keyboard
connecte
Communication problem
with PC keyboard
Check keyboard connection
with instrument switched off
validate instrument
Instrument has
been switched on
Set validation interval has
expired
1. Validate instrument
2. Contact Precisa Service
2. Reset time counter to
zero (see Sect. 5.5)
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8 Troubleshooting – Messages – Maintenance
8.3 QM support
Precisa AG can support you in your quality management (QM) measures:
Literature
The validation documentation will help you with your installation qualification
(IQ) and operating qualification (OQ).
Instrument-internal validation aids
The system test of the pH Meter checks that all the relevant assemblies are
functioning properly when the instrument is switched on. The result can be
produced directly as a system test report via the RS232 interface (see Sect.
5.5).
Calibration is a simple and necessary means of checking the functions of
the pH Meter and the electrodes connected to it. The determined calibration
data is checked according to certain criteria, can be assigned to a defined
electrode identification and can be stored together with it. When a defined
calibration interval has expired the instrument will inform you that the recalibration of the connected electrode is necessary. A description of the calibration parameters for the various modes can be found in Sect. 6.2.2 (pH).
You can use monitoring to have the instrument remind you automatically
about tasks which are due for validation purposes or service measures. Just
as for an expired calibration interval, these messages will also be protocolled
with each output of a measured value which has been determined since the
expiry of the due date even though the necessary measures have not yet
been taken.
With diagnose you can subject the various assemblies of the pH Meter to
further-going tests. This can help you to localize any faults which may occur.
This function can also be integrated in your validation measures. It is described in detail in Sect. 8.5.
The electrode test is a programmed sequence of various measurements for
checking the quality of the connected pH electrode. Sophisticated assessments help with the selective localization of an appearing problem. In Sect.
8.7 you will find an exact description of how to carry out such an electrode
test, a detailed interpretation of the possible test results as well as the appropriate measures for remedying the faults and preventing future ones.
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8 Troubleshooting – Messages – Maintenance
Test instruments
The Calibrated Reference can be used as test instrument for mV, pH, O, µS
and °C for both the pH960 pH Meter. When connected instead of a sensor it
allows a direct check of the functionality, basic accuracy and high impedance
of the pH Meter. In Sect. 8.6 you will find an exact description of such a test
run together with the test protocol to be drawn up.
The pH Simulator gives you the possibility of checking the measuring input
at any potentials between 0 and 2000 mV, pH values between 0 and 20 and
various temperatures between 0 and 100 °C with great accuracy.
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8 Troubleshooting – Messages – Maintenance
8.4 Validation
The checking and maintenance of the pH Meter can be carried out in 3 steps.
This list can be extended by the measures described in Sect. 8.3.
1. Checking the electronic components when the instrument is switched on.
2. Validation of the whole analytical system by wet chemistry.
3. pH Meter maintenance by Precisa Service.
8.4.1 Electronic tests
After the pH Meter has been switched on an electronic system test is carried
out automatically. The following display is seen:
The tests are documented in the system test report; this can be printed out
when the instrument is switched on: (see Sect. 5.4):
'di
pH 960
02104 5.781.0012
date 2002-07-09 15:32:00
RAM test
OK
EPROM test
OK
real time clock
OK
COMPort
OK
A/D converter
OK
LCD display
OK
==============
If one of these tests is not concluded with 'OK' then please contact Precisa
Service.
With a real time clock error you can try resetting the date and time. If the
test is then 'OK', you should check whether the stored methods and instrument configuration are still unchanged.
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8 Troubleshooting – Messages – Maintenance
8.4.2 Wet tests
Quality assurance standards such as GLP (Good Laboratory Practice) require
the regular validation of the analytical instruments. The reproducibility and accuracy of the instruments are checked.
Repeating the test at yearly intervals is normally adequate. However, depending upon the requirements, it may be necessary to carry out the test more
frequently, e.g. every 3 months or every 6 months.
AB No. 271: Validation of Precisa pH Meters.
The validation interval can be monitored by the pH Meter (see Sect. 5.5).
When the interval has expired the pH Meter will show the following message:
validate instrument
8.4.3 pH Meter maintenance
In the same way as monitoring the validation interval, the pH Meter can also
remind you that maintenance is due, e.g. by Precisa Service (see Sect. 5.5).
service is due
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8 Troubleshooting – Messages – Maintenance
8.5 Diagnosis
The pH Meter is equipped with a diagnosis program. This allows selective
checks of the functions of individual assemblies.
The diagnosis can be carried out directly after the instrument has been
switched on by pressing and holding down the <9> key. Only those tests
that you can carry out yourself are described below; the other functions are
reserved for Precisa Service personnel.
If one of the following tests is concluded with an error message, please note it
down and contact your local Precisa agency.
You are expressly warned against triggering any other functions other
than those listed and documented below. Improper use can disturb
the correct functioning of the pH Meter and may render it unusable.
diagnose
+ RAM Initialization
+ RAM Test
+ AD-Converter Test
+ LCD Display Test
:
+ Key
:
Test
RAM Initialization
Select: ACTMODE, MODES, SETUP, CONFIG,
ASSEMBLY, ALL
The initialization of the instrument memory can be a good idea if you want to
return parameter and configuration settings to their original condition. This
does not affect the instrument software itself, but only the above selection of
the corresponding user data. ACTMODE resets all method parameters of the
current measuring mode, MODES affects the method parameters of all
modes. With SETUP you can initialize the setup settings, with CONFIG all the
configuration data will be reset. ASSEMBLY functions, which can only be accessed via remote control, are reset here. The option ALL resets the whole
instrument memory to its original condition.
A memory initialization should only be triggered after careful consideration! It will permanently delete all the affected user data which must
then be reentered manually.
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8 Troubleshooting – Messages – Maintenance
When only certain configuration settings or method parameters are to be reset to their default values then the manual version is more suitable. Except
for a few special cases, all the corresponding default values can be set directly during input with the <CLEAR> key. In the other cases you will find the
default settings in these Instructions for Use in Sections 5 and 6.
RAM Test
This test checks the condition of the instrument memory without altering its
contents. A successful test is concluded with the message 'ram test ok'.
AD-Converter Test
The electronic components of the analog-digital converter are checked. At the
end the two messages 'ADC EEPROM Test ok' and 'ADC Int. ok x mS'
should appear. Instead of 'x' the message should contain a number between
15.0 and 25.0.
LCD Display Test
With this test you can check that the LCD display is functioning properly. It
consists of a sequence of individual tests which can be switched forward with
<QUIT>. The test can be halted with <ENTER> and canceled with
<MODE>.
Key Test
The correct functions of all the instrument keys can be checked here. After
the start a 3-fold beep will be heard (so that you can also test this straight
away) after which the instrument will respond to the pressing of each key by
displaying the corresponding key code. However, the <ON/OFF> key will still
switch off the pH Meter. This test is terminated by pressing the <CLEAR>
key twice.
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8 Troubleshooting – Messages – Maintenance
8.6 Checking the measuring input
During the calibration of a potentiometric measuring system not only the electrode is calibrated, i.e. measured potentials are assigned to particular measured quantities, but also faults which may be present at the measuring input,
e.g. inadequate high-impedance, will be temporarily compensated. In extreme cases this could mean that, despite successful calibration, unstable
and incorrect results are obtained. This is the reason why a comprehensive
validation concept should include the checking of the measuring amplifier.
The Calibrated Reference is a diagnostic tool which provides you or the
Precisa service technician with the possibility of checking the functions of the
pH Meter measuring amplifier (potential and temperature).
When using the Calibrated Reference please take the following points into
account:
1. The demands placed on the pH Meter vary strongly according to the
conditions under which it is used. This means that the requirement
profile and the corresponding volume of such additional checks can
only be defined individually.
2. For the reasons mentioned above the sensor cable should be included in the measuring amplifier check whenever this is possible, as
this is a possible source of high impedance interference.
3. This test is intended exclusively for the check of the pH960 pH Meter.
Therefore, all electrical connections, which are not used for the test,
must to be removed from the instrument (e.g. RS 232 or Remote connections). Otherwise the grounding of these connected devices would
cause large differences in step 6 of the following test. Such earth connections would lead to interferences during measurements in
grounded solutions. You may use this test to determine these earth
connections of connected devices.
4. The potentiometric measuring inputs (pH/ISE) are checked in Mode
U (mV). As the measurements of pH are nothing more than mathematically converted potential measurements, a separate check in the
pH mode is not necessary.
On the following pages you will find a protocol of such a test. You can copy
these two pages and use them as a form for filling in manually.
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8 Troubleshooting – Messages – Maintenance
Protocol of measuring amplifier check
Instr.:
.......... .......... Serial / Fabr.-No: .................. ID-No (if available):.........................
Test agent: ……………… Serial / Fabr.-No: ..................
Cal. date: .................................
calibrator (master)...................
SCS Cal. Serv. Reg. No: .........
Check carried out on:
ID-No (if available):.........................
checked by:.....................................
Type.................................................
Certificate No ..................................
...................... Name: ............................. Signature:..........................
Checked instrument
meets requirements:
yes
no
Decision:.........................................................................
Please read the notes on the following page first.
Checking U (mV)
Carry out on pH960
or on sensor
Remarks
Carry out
on 767
Enter theoreti- Enter value Difference Permitted OK
cal value from from pH960
difference2 ü
1
767 cover
display
1 Unscrew the cable at the plug- Place sensor Close cover
in head of the sensor, if possible. Otherwise insert cable
6.2150.040 from accessories
of 767 to socket 5 'pH/ISE'.
in sleeve
2 Press <MODE> to select
Sensor cable to mV value 5:
socket (5)
0 mV
3
Open cover
4
Sensor cable to (Actual value
socket (4)
from step 3)
Mode U (mV).
5
6 Connect grey banana plug of
Do not touch
767 cable 6.2150.020 to
sockets (4) earthing socket 13 of pH960 5; (6) during
black plug (screen) remains
measure.
open.
............. mV .......... mV ± 1.0 mV
....
mV value 5:
................. mV ............. mV .......... mV ± 1.5 mV
....
Diff. act. val.
step 3 and 4
3
............. mV .......... mV ± 1.0 mV
....
Sensor cable to mV value 6:
socket (6)
................. mV ............. mV .......... mV ± 2.5 mV
....
Sensor cable to (Actual value
socket (5);
from step 3)
767 cable
6.2150.020 to
socket (6)
Diff. act. val.
step 3 and 8
4
............. mV .......... mV ± 1.5 mV
....
Checking temperature (Pt1000)
Carry out on pH960
or on sensor
Remarks
Carry out
on 767
Enter theoreti- Enter value Difference Permitted OK
cal value from from pH960
difference2 ü
1
767 cover
display
1 Change to Mode T (°C) with
<MODE>.
No preference
for cover.
2 Use two banana cables
Connect to
sockets
(2) + (3):
................. °C
(1) + (3): 6
................. °C
(6.2150.000) to connect
temperature measuring input 8
to 767 5.
............. °C ...........°C ± 1.0 °C
............. °C ...........°C ± 1.0 °C
....
....
3 Remove cables and reconnect
sensors.
Preparation of the measuring amplifier check
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8 Troubleshooting – Messages – Maintenance
• Place Calibrated Reference on bench near sensor. Ensure that light reaches solar cell without interference (no shadows from cables or accessories). Switch on room lighting if necessary.
• The electrode cap must not necessarily be firmly screwed onto sockets (4), (5) and (6) of the
767; plugging it in is sufficient
• Unplug any temperature sensor that may possibly be connected; switch on pH Meter
• The decimal place in the digital display for mV (Mode U) and °C (Mode T) must be visible. If it is
not, activate it under CONFIG/ausxiliaries/last digit.
Remarks for the measuring amplifier check procedure
1
2
3
4
5
96
Wait until drift symbol disappears
The given permitted difference applies for normal room temperature (20 - 30 °C) and warmed up instruments. Alternatively these values can be determined from the technical specifications of the 767
and the pH960.
If the variation is too large try exchanging the electrode cable.
A larger short-time larger change is normal.
use adapter PN 3900-104 / PN 3900-105 from pH960 accessories
8 Troubleshooting – Messages – Maintenance
8.7 pH electrode test
EL.TEST
1
With the pH Meter you can carry out an automatic pH electrode test which al-
lows the quality of the electrode used to be evaluated. As the result you will
obtain various information about the characteristic measuring properties of
your pH electrode (slope, response time, drift, streaming potential). The concluding evaluation of the electrode is carried out by checking the results obtained against preset tolerances.
These tolerances are stored in the pH Meter for the three most frequently
used types of Precisa pH electrodes: standard electrodes, gel electrodes
and non-aqueous electrodes. You can also define your own limits. The
specific classification of the electrode system is defined by the reference system used. You find overview for these electrode types and the corresponding
tolerances on page 101.
In the electrode test faulty electrodes frequently show certain combinations of
measured results which lie outside the preset limits. This permits more detailed information to be given about possible causes and recommended
measures.
8.7.1 Preparations
Buffers
You need faultless pH 4, pH 7 and pH 9 buffers for carrying out the electrode
test. We recommend the use of suitable Precisa buffers. In principle the electrode test can also be carried out with any of the stored sets of buffers which
contain buffers with these values. The set of buffers used must be set in the
calibration parameters (see also Sect. 6.2.2):
PARAMETER pH
+ calibration parameter
+ buffer type
If an electrode test is started with a set of buffers which does not contain the
necessary buffers then the following error message will appear:
buffers unsuitable
TIP !
Particularly with buffer pH 9 you should make certain that it is in a faultless
condition. By absorption of CO2 from the atmosphere this buffer can easily
vary from its specified pH values and therefore produce incorrect test results.
Stirrer
You require a stirrer for the test.
With a 101 Magnetic Stirrer the test is fully automated. You just have to
change the buffers. Set the stirring rate at
PARAMETER pH/measuring parameters/stirrer: ON
stirring rate
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8 Troubleshooting – Messages – Maintenance
The stirring rate should be set so that the stirring action is powerful but without the formation of bubbles (avoidance of CO2 entrainment).
For other connected stirrers this measuring parameter stirrer must be set
to 'ON'.
If an unconnected stirrer is used then you will have to switch it on and off
manually during the test. A request will be made at the appropriate places
during the test.
Printer
If you want to print out either a full or short test report then a printer must be
connected (see Sect. 2.3) and its configuration set properly (see Sect. 5.6
and 5.7).
Parameter settings
Before the start of the electrode test it may be necessary to adapt the electrode test parameters. These parameters are described in Section 6.2.7.
Temperature
Please ensure that the whole electrode test is carried out at a constant temperature. As the temperature has a great influence on the response time you
should work at room temperature (25 °C) if possible as the preset tolerances
are set for this temperature.
In the following section the exact electrode test procedure is described. It is
assumed that a temperature sensor is connected: if not, you must determine
the measuring temperature manually and enter it at the start of the electrode
test when the request for it appears on the display.
8.7.2 Procedure
The whole pH electrode test is dialog guided; this means that you will be requested to carry out any activity which is required. The sequence is as follows: the pH electrode is first immersed in the pH 9 buffer and its potential is
measuring for three minutes under stirring followed by one minute without stirring. The same measurements are then repeated at pH 4 and pH 7. If no controllable stirrer is connected you will be requested to switch the stirrer on and
off at the required times.
In order to obtain realistic response times the electrode should be immersed
in each buffer at about the same time as the measurement is started and it
should be positioned directly above the stirrer which has already been
switched on.
The pH Meter in the pH mode should be in the normal working condition
(measured value display). Otherwise switch to this mode with <MODE>.
EL.TEST
1
98
1
Start pH electrode test
• The electrode test is started from the pH measured value display with <EL.TEST>.
8 Troubleshooting – Messages – Maintenance
2
(Enter temperature)
• If no temperature sensor is connected then the measuring
temperature of the buffers must be entered here. This should
be the same for all buffers.
3
Immerse electrode in pH 9 buffer
• Immerse the electrode in the pH 9 buffer and immediately
press <ENTER>.
ENTER
• The instrument now counts down from 239 to 0 seconds.
• If a 101 stirrer is connected and configured (see Sect. 8.7.1)
then it will be switched off automatically after 3 minutes. Otherwise you will be requested to switch off the stirrer; this request must be confirmed with <ENTER>.
• If a temperature sensor is connected the temperature measurement will then be carried out.
4
ENTER
Immerse electrode in pH 4 buffer
• Immerse the electrode in the pH 4 buffer and immediately
press <ENTER>.
• Further procedure as for the pH 9 buffer.
5
ENTER
Immerse electrode in pH 7 buffer
• Immerse the electrode in the pH 7 buffer and immediately
press <ENTER>.
• Further procedure as for the pH 9 buffer.
6
Evaluation of the pH electrode and report output
• The electrode evaluation will then appear on the display. If
applicable the report will also be printed out on a connected
printer.
• If interference occurs the electrode test may be terminated.
Such interference is also shown on the display and noted in
the report (see Sect. 8.7.4)
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8.7.3 Results
The following graph shows the potential of the pH electrode as a function of
time during the electrode test for a buffer in diagram form:
Fig. 8:
Diagram showing changes in potential during an electrode test
The evaluation of the pH electrode is made according to the following criteria.
These measured and calculated values are listed in the printed report:
Streaming potential dU (unstirred - stirred)
This is the absolute difference between the measured potentials in the stirred
(after 3 min) and unstirred solution. It is determined at each pH, but is initially
most significant for the pH 9 buffer.
Drift
The absolute drift in the stirred solution (after 3 min) is determined at each pH
and used to calculate the total.
Slope
Just as in a calibration, for each pH combination (pH 4/7, 7/9 and 9/4) the
electrode slope, pH(0) and the offset potential Uoff are determined in the
stirred solution.
Response time t(1mV)
Time after which the measured potential is within 1 mV of the potential determined in the stirred solution after three minutes.
Offset potential Uoff
The offset potential Uoff, which is determined together with the slope and
pH(0), is tested once against a preset limit and is not included in the evaluation.
The following table lists the preset tolerances for the three types of electrode:
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8 Troubleshooting – Messages – Maintenance
excellent
electrode
good
electrode
passing
electrode
= 2.5
= 2.0
96.5 = s = 101
= 45
= 3.0
= 2.5
96 = s = 102
= 50
= 4.0
= 3.0
95 = s = 103
= 60
-15 = Uoff = 15
Electrode type: standard
Streaming potential dU [mV]
Total drift [mV]
Slope s [%]
Response time [s]
Offset potential Uoff [mV]
Electrode type: gel => all (reference-) electrodes filled with Idrolyte
Streaming potential dU [mV]
= 3.0
= 3.5
Total drift [mV]
= 2.5
= 3.0
Slope s [%]
96.5 = s = 101
96 = s = 102
Response time [s]
= 60
= 75
= 4.5
= 4.0
95 = s = 103
= 90
Offset potential Uoff [mV]
-15 = Uoff = 15
Electr. type: non-aqueous => all (reference-) electrodes filled with TEABr or LiCl in ethanol
Streaming potential dU [mV]
=3
= 4.5
=6
Total drift [mV]
=5
=7
=9
Slope s [%]
88 = s = 120
80 = s = 130
70 = s = 140
Response time [s]
= 60
= 75
= 90
Offset potential Uoff [mV]
-10 = Uoff = 70
The tested pH electrode is given that evaluation for which it fulfills all the criteria. If one of the tolerances for a usable (passing) electrode is not observed
then the electrode test will be concluded with the message 'electrode out
of limits.' in the report. If further test criteria are also not fulfilled then the
electrode test evaluation will be 'electrode test not passed'. In addition a more specific error message will be shown on the display and will also
be included in the report (see following section).
TIP !
Instead of the stored tolerances for most Metrohm electrodes you can set
your own values (see Sect. 6.2.7). This may be helpful for special applications
if, for example, other quality requirements are placed on the pH electrode or
work is carried out with a reference electrode which displaces the offset potential Uoff beyond the required –15 to +15 mV (standard and gel electrodes).
101
8 Troubleshooting – Messages – Maintenance
8.7.4 Messages and measures
For the test results 'passing electrode' and 'electrode out of limits' the following recommendations for improving the quality of the electrode
can be given:
Result
Measure
passing electrode
Clean diaphragm
electrode out of limits
Clean diaphragm and/or regenerate the glass membrane;
check reference system
The following general information should be taken into consideration when
evaluating the electrode test results:
• With separate measuring and reference electrodes the pH electrode is
not always the cause of unexpectedly poor test results. This is why you
should also check the condition of the reference electrode (see Sect.
8.7.5).
• If the tested pH electrode has been given a lower evaluation only because of its slope being inadequate then you should compare the individual slopes at pH 4/7 and pH 7/9. If these values are different then
repeat the electrode test using a fresh pH 9 buffer. Only then can you
conclude that there is an electrode problem.
• A correct outflow of the inner electrolyte causes only a minimum
potential drop when the stirrer is turned of (s. Fig. 8). A large drop indicates a too small outflow - the diaphragm is blocked. If you obtain a
potential step-up, the outflow is too high and should be corrected.
• Under certain conditions, e.g. very low relative humidity, plastic floor
coverings or clothing made from synthetic materials, the pH electrode
can be affected by electrostatic discharges. The results are high
drift values and correspondingly poor electrode test results. Such
problems can be avoided by the user wearing e.g. an antistatic bracelet.
In addition to the evaluation of the electrode quality described above, the
measured values are also checked to see if they have exceeded certain tolerances. In such cases the electrode test is concluded with the following message on the display:
electrode test not passed
More specific error messages will also be shown and included in the report.
The following table lists these tests, the resulting messages and recommended measures for remedying their possible causes. These measures are
described in detail in Section 8.7.5.
The first two tests are carried out after the measurement in the pH 9 buffer
and the electrode test then stopped if necessary.
102
8 Troubleshooting – Messages – Maintenance
Test criterion
Message
Measure
pH 9: absolute drift in stirred
solution > 1 mV/min
problem
Clean diaphragm and/or
regenerate the glass membrane.
pH 9:
-10 mV < U(unstirred) < 10 mV
AND
sum of abs. drift values after 1, 2,
3 and 4 min < 12 mV/min
short circuit
Replace electrode (short circuit
or crack in glass membrane).
2 slopes do not meet the
conditions for a passing
electrode
check buffer/
electrode
Repeat test using correct
buffers.
Electrode poor as streaming
potential dU is too high
bad diaphragm
Clean diaphragm.
All slopes meet conditions for
passing electrode
reference not
matching
Repeat with suitable reference
system; replace contaminated
reference electrolyte. If
necessary select electrode type
'own' and adapt the Uoff limits.
All slopes do not meet conditions
for passing electrode
partial short
circuit
Check temperature sensor or
enter correct temperature. If this
does not help then replace pH
electrode.
A response time does not meet
the criterion for passing electrode
glass
membrane/
reference
Regenerate glass membrane
and/or clean diaphragm.
AND
Uoff outside the preset limit
8.7.5 Care and maintenance of pH glass electrodes
General
• A combined pH electrode must be filled with the correct reference
electrolyte, e.g. with c(KCl) = 3 mol/L.
• The reference electrolyte chamber should be completely filled with
clean electrolyte.
• The reference electrolyte filling opening must remain open during the
measurement and be closed during storage.
• There should be no air bubbles in the inner or reference electrolyte.
• All cable connections should be clean and dry.
Storage
• Combined glass electrodes should be stored in the reference electrolyte (c(KCl) = 3 mol/L). If the electrode is stored in water then AgCl will
precipitate out in the diaphragm!
103
8 Troubleshooting – Messages – Maintenance
• Separate glass electrodes should be stored in distilled water.
Cleaning the diaphragm
• After measurements in solutions with low chloride concentration (precipitated AgCl in the diaphragm which is colored dark brown): place
electrode overnight in a concentrated ammonia solution, rinse with water and replace the reference electrolyte.
• After measurements in protein-containing solutions: place electrode in
a solution of 5% pepsin in c(HCl) = 0.1 mol/L for several hours; the
best effects are obtained at a temperature of 38 °C. Then rinse thoroughly with water and replace the reference electrolyte.
• After measurements in sulfide-containing solutions (Ag2S in diaphragm, which has a dark color): immerse electrode in freshly prepared, slightly acidic 7% thiourea solution for several hours. Then rinse
with water and replace the reference electrolyte.
• If the electrode is contaminated by organic compounds: immerse electrode in chromosulfuric acid for approx. 15 minutes at 80 °C. Then
rinse with water and replace the reference electrolyte.
• Note: Ultrasonic cleaning can destroy the electrode!
Care of the glass membrane
• When carrying out measurements in non-aqueous media the electrode
should be hydrated between measurements.
• Regenerating the glass membrane: immerse the glass membrane in
either a 10% solution of ammonium hydrogen fluoride (NH4HF2) for one
minute or in 40% HF for a few seconds. Warning: HF is a strong skin
poison! Do not use glass vessels! After the etching process rinse in
H2O:HCl = 1:1 for approx. 10 seconds. Then rinse the electrode with
water and let it stand in the storage solution for 24 h.
104
9 Annex
9 Annex
In this section you will find the most important technical data of the pH Meter,
a description of evaluation principles, dialog structures, buffer tables, a list of
standard accessories and optional accessories as well as warranty and declarations of conformity.
9.1 Technical data
Provided that nothing to the contrary is mentioned, the published values represent the typical data of the pH960 pH Meter.
9.1.1 Measuring modes
Measuring mode
Prim. measured
quantity
Sec. measured
quantity
pH
T
pH
Temperature
T
Potential
U
9.1.2 Measuring inputs
Potentiometric
for pH and potential
• 1 high-impedance measuring input for pH, redox and ISE electrodes
• 1 reference input for separate reference electrode
Input resistance
Offset potential
> 1012 Ohm
< 10-12 A
(under reference
conditions)
Temperature
Also for automatic temperature compensation
• 1 measuring input for temperature sensors (Pt1000 or NTC)
NTC characteristics configurable
Default values:
R(25°C) = 30000 Ohm / B25/50 = 4100
Measuring interval
Measuring cycle
100 ms for all measuring modes
105
9 Annex
9.1.3 Measuring input specifications
Measuring
mode
Measuring range
pH
-20.000 .. +20.000 pH
Temperature
-150 °C .. +250 °C (Pt1000)
-20 °C .. +250 °C (NTC)
Potential
1
2
-2200 mV .. +2200 mV
Resolution
0.001 pH
Measuring accuracy 1)
± 0.003 pH
0.1 °C
± 0.2 °C
(Pt1000/-20°C...+150°C)
0.1 mV
± 0.2 mV
) ±1 digit, without sensor error, under reference conditions
) for single charged Ions
9.1.4 Interfaces
RS232 connection
RS232
Hardware and software handshake
for printer and remote control
MSB connections (MSB = Serial Bus)
Stirrer
Connection of max. 1 stirrer
Stirrer control: manual on/off, or
automatic during measuring sequence
Rate selectable in 15 steps
Barcode / Keyboard connection
PC keyboard
PS/2 PC keyboard
Barcode
Barcode reader with PS/2 interface
9.1.5 Power supply
Power unit
12 V ±1%, 1A
Power consumption
5 W (without external loads)
The following current consumers are allowed:
106
Stirrer at MSB connection
< 200 mA, 12 V
Barcode + Keyboard
< 250 mA, 5 V
9 Annex
9.1.6 Safety specifications
Instrument pH960
Standards fulfilled:
- EN/IEC 61010-1 (protection class 3)
9.1.7 Electromagnetic compatibility (EMC)
Emission
Standards fulfilled:
- EN/IEC 61326-1
- EN 55022
- EN/IEC61000-3-2
- EN/IEC61000-3-3
Immunity
Standards fulfilled:
- EN/IEC 61326-1
- EN/IEC 61000-4-2
- EN/IEC 61000-4-3
- ENV 50204
- EN/IEC 61000-4-4
- EN/IEC 61000-4-5
- EN/IEC 61000-4-6
- EN/IEC 61000-4-8
- EN/IEC 61000-4-11
- EN/IEC 61000-4-14
9.1.8 Ambient temperature
Nominal
working range
+5 °C...+45 °C (max. 85% rel. humidity)
Storage
-20 °C...+60 °C
Transport
-40 °C...+60 °C
9.1.9 Reference conditions
Ambient temperature
+25 °C (±3 °C)
Rel. humidity
≤ 60 %
Warmed-up condition
instrument in operation for at least 30 min
Data validity
after balancing
9.1.10 Dimensions
Housing material
polybutylene terephthalate (PBTP)
Keyboard material
Polyester
Display cover material
Glass
Width
305 mm
Height (without stand)
55 mm
Height (with stand)
410 mm
Depth
170 mm
Weight (without stand)
1378 g
107
9 Annex
9.2 Evaluation
9.2.1 pH calibration
pH calibration is used to assign the potentials measured at the pH electrode
to the corresponding pH values. This relationship is known theoretically and is
described by the Nernst equation. For pH measurement it can be simplified
to:
U = U pH =0 − U N ⋅ pH
where
T : absolute temperature in K
R : ideal gas constant
F : Faraday-Konstante
UpH=0 is the ordinate intercept at pH
=
0. Its value depends on the construction of the electrode. The theoretical
Nernst constant UN is temperature-dependent and is e.g. 59.16 mV at 25 °C.
This means that theoretically, i.e. with a standard pH glass electrode (inner
electrolyte 3 M KCl: pH 7.0; Ag/AgCl reference system), at pH 7.0 a potential
of 0 mV should be measured. This represents the so-called zero point of the
electrode. The graphical plot of further U/pH pairs of values within the normal
pH range then provides a linear relationship according to the above equation
whose slope is -UN.
Fig. 9:
Theoretical U/pH relationship
In fact this U/pH curve is usually different. The offset potential of the electrode
(Uoff = U at pH 7.0) may not be zero as a result of the asymmetry potential at
the glass membrane, a contaminated inner electrolyte or an unsuitable reference system. The slope can also differ slightly from UN.
108
9 Annex
As these variations describe the condition of the pH electrode and are subject
to variation with time this means that, depending on the accuracy required, a
regular pH calibration is necessary. This calibration provides a new description of the relationship between the electrode potential and the measured pH
value:
Fig. 10: 3-Point pH calibration
pH(0) and slope are outputted by the pH Meter as calibration data. In this
case the slope (e.g. 99.5%) is a relative quantity which refers to the temperature-specific value of the Nernst constant. It is given with a positive sign,
which is why the following explanations are extended by including the negative sign.
Using this data the calibration curve can be described as follows:
U = − Slope ⋅ U N ⋅ ( pH − pH (0) )
or
pH = pH (0) −
U
Slope ⋅ U N
109
9 Annex
The calculation of the calibration data depends on the number of pH buffers
used:
1-Point calibration
Slope :
The theoretical slope value of 100.0% is used.
pH (0)
= pH 1 −
U1
− Slope ⋅ U N
2-Point calibration
(U 2 − U 1 )
Slope
=
pH (0)
= pH −
( pH 2 − pH 1 )
⋅
1
−U N
U
− Slope ⋅ U N
; pH , U = mean value
3- and more point calibration
With at least 3 calibration buffers a compensation curve according to the
principles of the smallest mean-square error (linear regression) will be calculated.
Slope
=
∑ ( pH
i
i
)(
− pH ⋅ U i − U
∑ (pH
i
− pH
)
2
)
⋅
1
−UN
i
pH (0)
Variance =
110
U
− Slope ⋅ U N
= pH −
∑ (U
i
− U i ,calculated )
i
n−2
2
; n = no. of measuring points
9 Annex
Notes
For a pH calibration at least two or more different buffers should be used;
these should cover the intended measuring range (DIN 19268). For example,
you can obtain Precisa buffer solutions for pH 4, 7 and 9 as ready-to-use
solutions or concentrates (see Optional Accessories, Sect. 9.6).
A pH electrode is an ion-selective electrode which responds to hydrogen ions
(H+) with great selectivity. This is the reason why the above linear relationship
between the measured potential U and the pH value based on it can be assumed. A variation may be caused by the so-called alkali error. This describes the interference by high concentrations of alkali ions (e.g. 0.1 M Na+)
which can occur at high pH values (> pH 12).
The temperature compensation of the pH Meters during a pH measurement for the calculation of the pH value is based on a temperature-corrected
slope (conversion via the definition of the Nernst constant UN, see p. 108).
This method is based on the assumption that the intercept of all theoretical
Nernst slopes lies at pH 7.0 and 0 mV (isothermal intercept point).
However, this is not always the case. The measuring uncertainty increases
with the temperature difference between calibration and measurement. Therefore, calibration and measurement should be performed at the same temperature wherever a high degree of accuracy is required. In this case DIN
19268 also stipulates that calibration and measurement are to be carried out
at the same constant temperature.
The temperature compensation considers only the temperature dependence
of the Nernst slope. In addition, the pH values of buffers and samples are
also temperature dependent. The temperature dependence of the buffer is
corrected by means of the stored buffer series (s. Sect. 9.4). But no such information is usually given for the sample. Therefore, the pH should be measured at the 'original' sample temperature instead of adjusting the sample
temperature to the buffer temperature. For high accuracies it is recommended that you calibrate at the samples temperature. During the calibration
take care of a correct correlation of the temperature specific buffer pH values.
111
9 Annex
9.3 Menu structures
The menu structures of the instrument configuration and the method parameters of all operating modes are shown on the following pages.
This so-called instrument tree can also be used to control the pH Meter via
the serial interface
9.3.1 Instrument configuration
CONFIG
¦
+
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
+
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
+
¦
¦
¦
:
112
report
+ id1
+ id2
+ report id
+ instrument id
+ date & time
+ method
+ electrode id
+ signature
+ line feed
print meas.value
+ print crit -----
¦
¦
+
¦
¦
¦
¦
+
¦
¦
+
¦
¦
¦
+
store meas.value
+ store crit -----
+
immediate
time
drift
plot
+
+
+
+
+
+
+
+
+
+
+
date & time
report header
calibration report
date & time
report header
calibration report
time interval
stop time
date & time
report header
calibration report
time interval
time scale
time scale label
stop time
OFF
immediate, drift, OFF
time
- time interval
+ stop time
9 Annex
CONFIG (Fortsetzung)
:
:
+
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
+
¦
¦
¦
¦
¦
+
¦
¦
¦
¦
¦
¦
+
auxiliaries
+ run number
+ last digit
+ dialog
+ display
+ LCD off after
+ date
+ time
+ time zone
+ temp.sensor --
¦
¦
+
+
+
+
+
temp.unit
device label
beep
program
monitoring
+ validation
¦
+
+
Pt1000
NTC - R(25 °C)
+ B value
-------
ON
service ---------system test report
ON
+
-
time interval
time counter
next service
peripheral units
+ character set
+ dosimat
+ stirrer
+ keyboard
+ barcode
RS232 settings
+ baud rate
+ data bit
+ stop bit
+ parity
+ handshake
113
9 Annex
9.3.2 Method parameters in the pH mode
PARAMETER pH
¦
+
¦
¦
¦
¦
¦
¦
¦
+
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
¦
+
¦
¦
¦
¦
+
¦
¦
+
¦
¦
¦
¦
¦
¦
¦
¦
+
measuring parameters
+ electr.id
+ drift pH
+ temperature
+ method
+ delta measurement - ON --- reference pH
+ stirrer
---- ON ---- stirring rate
+ control - stirring rate
calibration parameters
+ prestir pause
+ temperature
+ stir time
+ drift
+ poststir pause
+ report
+ cal.interval
+ no.of buffers
+ buffer type ---- Precisa, Metrohm, NIST, DIN, ...
¦
+ special - pH buffer 1
¦
¦
¦
¦
¦
¦
¦
+
+
+
+
+
low lim.slope
up lim.slope
low lim.pH(0)
up lim.pH(0)
offset Uoff state
own
mixed
-
ON
:
+
:
+
:
+
buffer 5
-
offset Uoff
pH buffer n
own buffer 1
own buffer 5
buffer 1
limits pH
+ state
-----
ON
---+
+
+
u.limit
u.hyst.
l.limit
l.hyst.
limits T
+ state
-----
ON
---+
+
+
u.limit
u.hyst.
l.limit
l.hyst.
plot parameters
+ left mar. pH
+ right mar. pH
+ left marg.T
+ right marg.T
pH
pH
pH
pH
preselections
+ req.ident
electrode test
+ electrode type
¦
+
+
114
¦
¦
+
¦
¦
+
temperature
report
+
standard, gel, non-aqu.
own ---- excellent electrode
+ good electrode
+ passing Elektrode
+ l.limit Uoff
+ u.limit Uoff
9 Annex
9.3.3 Method parameters in the T mode
PARAMETER T
¦
+
¦
¦
¦
¦
¦
¦
¦
¦
¦
+
¦
¦
+
¦
¦
¦
+
measuring parameters
+ electr.id
+ drift
+ method
+ delta measurement - ON -- reference
+ stirrer
----- ON -- stirring rate
+ control - stirring rate
+ prestir pause
+ stir time
+ poststir oause
limits T
+ state
----- ON --- u.limit
+ u.hyst.
plot parameters
+ l.limit
+ left mar.
+ l.hyst.
+ right mar.
preselections
+ req.ident
9.3.4 Method parameters in the U mode
PARAMETER U
¦
+
¦
¦
¦
¦
¦
¦
¦
¦
¦
+
¦
¦
+
¦
¦
¦
+
measuring parameters
+ electr.id
+ drift
+ method
+ delta measurement - ON -- reference
+ stirrer
----- ON -- stirring rate
+ control - stirring rate
+ prestir pause
+ stir time
+ poststir oause
limits U
+ state
----- ON --- u.limit
+ u.hyst.
plot parameters
+ l.limit
+ left mar.
+ l.hyst.
+ right mar.
preselections
+ req.ident
115
9 Annex
9.4 Stored buffer series
For automatic buffer recognition during pH calibration the temperaturedependent pH values of several common pH buffers are stored in the pH960
pH Meter. Apart from the Preicsa buffer solutions PN 3900-04x other reference and technical buffers are also included in the tables.
The following tables provide an overview of the stored pH(T) series. Buffers
marked with an * are not taken into account during automatic buffer recognition if one of the complete sets of buffers is selected as the buffer type. However, all the buffers listed can be selected to give a new combination under
PARAMETER pH/calibration parameters/buffer type:
mixed
(see Sect. 6.2.2).
Precisa/Metrohm
Temp.
(°C)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
116
Met4
Met7
Met9
pH 4.00 pH 7.00 pH 9.00
3.99
3.99
3.99
3.99
3.99
4.00
4.00
4.01
4.02
4.03
4.04
4.06
4.07
4.09
4.11
4.13
4.15
4.18
4.20
4.23
7.11
7.08
7.06
7.04
7.02
7.00
6.99
6.98
6.98
6.97
6.97
6.97
6.97
6.98
6.98
6.99
7.00
7.00
7.01
7.02
9.27
9.18
9.13
9.08
9.04
9.00
8.96
8.93
8.90
8.87
8.84
8.81
8.79
8.76
8.74
8.73
8.71
8.70
8.68
8.67
NIST
NIST1
pH 1
NIST4
pH 4
NIST7
pH 7
NIST9
pH 9
NIST13
pH 13
1.67
1.67
1.67
1.68
1.68
1.69
1.69
1.70
1.70
1.71
1.72
1.72
1.73
1.74
1.75
1.77
1.78
1.79
1.81
4.01
4.00
4.00
4.00
4.00
4.01
4.02
4.03
4.04
4.05
4.06
4.08
4.09
4.11
4.13
4.15
4.16
4.19
4.21
4.23
6.98
6.95
6.92
6.90
6.88
6.87
6.85
6.84
6.84
6.83
6.83
6.83
6.84
6.84
6.85
6.85
6.86
6.87
6.88
6.89
9.46
9.39
9.33
9.28
9.23
9.18
9.14
9.11
9.08
9.05
9.02
8.99
8.96
8.94
8.92
8.90
8.89
8.87
8.85
8.83
13.42
13.21
13.00
12.81
12.63
12.45
12.29
12.13
11.98
11.84
11.71
11.57
11.45
-
9 Annex
DIN
Fisher
Temp.
(°C)
DIN1
pH 1
DIN3
pH 3
DIN4
pH 4
DIN7
pH 7
DIN9
pH 9
DIN12
pH 12
Fis4
pH 4
Fis7
pH 7
Fis10
pH 10
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
1.08
1.08
1.09
1.09
1.09
1.09
1.10
1.10
1.10
1.10
1.11
1.11
1.11
1.11
1.11
1.12
1.12
1.12
1.13
-
3.10
3.08
3.07
3.06
3.05
3.05
3.04
3.04
3.04
3.04
3.04
3.04
3.04
3.04
3.05
3.06
3.07
-
4.67
4.66
4.66
4.65
4.65
4.65
4.65
4.66
4.66
4.67
4.68
4.69
4.70
4.71
4.72
4.74
4.75
4.77
4.79
-
6.89
6.86
6.84
6.82
6.80
6.79
6.78
6.77
6.76
6.76
6.76
6.76
6.76
6.76
6.76
6.77
6.78
6.79
6.80
-
9.48
9.43
9.37
9.32
9.27
9.23
9.18
9.13
9.09
9.04
9.00
8.97
8.92
8.90
8.88
8.86
8.85
8.83
8.82
-
13.37
13.15
12.96
12.75
12.61
12.44
12.29
12.13
11.98
11.84
11.69
11.56
11.43
11.30
11.19
11.08
10.99
-
4.01
3.99
4.00
3.99
4.00
4.00
4.01
4.02
4.03
4.04
4.06
4.07
4.09
4.11
4.13
4.14
4.16
4.18
4.21
4.23
7.13
7.10
7.07
7.05
7.02
7.00
6.99
6.98
6.97
6.97
6.97
6.97
6.98
6.99
7.00
7.02
7.03
7.06
7.08
7.11
10.34
10.26
10.19
10.12
10.06
10.00
9.94
9.90
9.85
9.81
9.78
9.74
9.70
9.68
9.65
9.63
9.62
9.61
9.60
9.60
Fluka Basle
Mettler Toledo
Temp.
(°C)
FBS4
FBS7
FBS9
MT2
MT4
MT7
MT9
MT11
pH 4
pH 7
pH 9
pH 1
pH 4
pH 7
pH 9
pH 11
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
4.01
4.00
4.00
4.00
4.00
4.01
4.01
4.02
4.03
4.04
4.06
4.07
4.09
4.11
4.13
4.14
4.16
4.18
4.21
4.23
7.11
7.08
7.05
7.02
7.00
6.98
6.97
6.96
6.95
6.94
6.94
6.93
6.93
6.93
6.94
6.94
6.95
6.96
6.97
6.98
9.20
9.15
9.10
9.05
9.00
8.96
8.91
8.88
8.84
8.80
8.77
8.74
8.71
8.69
8.67
8.65
8.63
8.61
8.60
8.59
2.03
2.02
2.01
2.00
2.00
2.00
1.99
1.99
1.98
1.98
1.98
1.98
1.98
1.98
1.99
1.99
2.00
2.00
2.00
-
4.01
4.01
4.00
4.00
4.00
4.01
4.01
4.02
4.03
4.04
4.06
4.08
4.10
4.13
4.16
4.19
4.22
4.26
4.30
4.35
7.12
7.09
7.06
7.04
7.02
7.00
6.99
6.98
6.97
6.97
6.97
6.98
6.98
6.99
7.00
7.02
7.04
7.06
7.09
7.12
9.52
9.45
9.38
9.32
9.26
9.21
9.16
9.11
9.06
9.03
8.99
8.96
8.93
8.90
8.88
8.85
8.83
8.81
8.79
8.77
11.90
11.72
11.54
11.36
11.18
11.00
10.82
10.64
10.46
10.28
10.10
-
117
9 Annex
Merck
Temp.
(°C)
Mer1*
pH 1
Mer2
pH 2
Mer3*
pH 3
Mer4
pH 4
Mer4.66*
pH 4.66
Mer5*
pH 5
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
0.96
0.99
0.99
0.99
1.00
1.01
1.01
1.01
1.01
1.01
1.01
1.02
1.02
1.02
1.02
1.02
1.02
1.02
1.02
-
2.01
2.01
2.01
2.00
2.00
2.00
2.00
2.00
2.00
2.00
2.00
2.00
2.00
2.00
2.01
2.01
2.01
2.01
2.01
-
3.05
3.05
3.03
3.01
3.00
3.00
3.00
3.00
2.98
2.98
2.97
2.97
2.97
2.97
2.97
2.97
2.97
2.97
2.96
-
4.05
4.04
4.02
4.01
4.00
4.01
4.01
4.01
4.01
4.00
4.00
4.00
4.00
4.00
4.00
4.00
4.00
4.00
4.00
4.00
4.68
4.68
4.67
4.67
4.66
4.66
4.66
4.66
4.67
4.68
4.68
-
5.06
5.05
5.02
5.01
5.00
5.00
5.00
5.00
5.00
5.01
5.01
5.03
5.04
5.05
5.05
5.08
5.10
5.12
5.14
-
Mer6* Mer6.88*
pH 6
pH 6.88
6.04
6.02
6.01
6.00
6.00
6.02
6.03
6.03
6.04
6.05
6.06
6.08
6.10
6.11
6.12
6.15
6.17
6.21
6.24
-
6.98
6.95
6.92
6.90
6.88
6.86
6.86
6.85
6.84
6.84
6.84
6.84
6.84
6.84
6.84
6.85
6.86
6.87
6.88
-
Merck
118
Temp.
(°C)
Mer7
Mer8*
Mer9
Mer11*
Mer12
Mer13*
pH 7
pH 8
pH 9
Mer9.22* Mer10*
pH 9.22
pH 10
pH 11
pH 12
pH 13
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
7.13
7.07
7.05
7.02
7.00
6.98
6.98
6.96
6.95
6.95
6.95
6.95
6.96
6.96
6.96
6.96
6.97
6.98
7.00
7.02
8.15
8.10
8.07
8.04
8.00
7.96
7.94
7.92
7.90
7.88
7.85
7.84
7.83
7.82
7.80
7.79
7.78
7.77
7.75
-
9.24
9.16
9.11
9.05
9.00
8.95
8.91
8.88
8.85
8.82
8.79
8.76
8.73
8.72
8.70
8.68
8.66
8.65
8.64
-
9.46
9.40
9.33
9.28
9.22
9.18
9.14
9.10
9.07
9.04
9.01
8.99
8.96
8.95
8.93
8.91
8.89
8.87
8.85
-
10.26
10.17
10.11
10.05
10.00
9.94
9.89
9.84
9.82
9.78
9.74
9.71
9.67
9.65
9.62
9.59
9.55
9.52
9.49
-
11.45
11.32
11.20
11.10
11.00
10.90
10.81
10.72
10.64
10.56
10.48
10.47
10.45
10.32
10.19
10.13
10.06
10.00
9.93
-
12.58
12.41
12.26
12.10
12.00
11.88
11.72
11.67
11.54
11.44
11.33
11.19
11.04
10.97
10.90
10.80
10.70
10.59
10.48
-
13.80
13.59
13.37
13.18
13.00
12.83
12.67
12.59
12.41
12.28
12.15
11.95
11.75
11.68
11.61
11.50
11.39
11.27
11.15
-
9 Annex
Beckman
Temp.
(°C)
Bec4
pH 4
Bec7
pH 7
Bec10
pH 10
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
4.00
4.00
4.00
4.00
4.00
4.00
4.01
4.02
4.03
4.05
4.06
4.08
4.09
4.11
4.12
4.14
4.16
4.18
4.19
4.21
7.12
7.09
7.06
7.04
7.02
7.00
6.99
6.99
6.98
6.98
6.97
6.98
6.98
6.99
6.99
7.00
7.00
7.01
7.02
7.03
10.32
10.25
10.18
10.12
10.06
10.01
9.97
9.93
9.89
9.86
9.83
-
Radiometer
Temp. Rad1.09* Rad1.68* Rad4.01 Rad6.84* Rad7.00 Rad7.38* Rad9.18 Rad10.01*
(°C)
pH 1.09 pH 1.68 pH 4.01 pH 6.84
pH 7
pH 7.38 pH 9.18 pH 10.01
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
1.082
1.085
1.087
1.089
1.091
1.094
1.096
1.098
1.101
1.103
1.106
1.108
1.111
1.113
1.116
1.119
1.121
1.124
1.127
-
1.666
1.668
1.670
1.672
1.675
1.679
1.683
1.688
1.694
1.700
1.707
1.715
1.723
1.732
1.743
1.754
1.765
1.778
1.792
-
4.000
3.998
3.997
3.998
4.001
4.005
4.011
4.018
4.027
4.038
4.050
4.064
4.080
4.097
4.116
4.137
4.159
4.183
4.210
4.240
6.984
6.951
6.923
6.900
6.881
6.865
6.853
6.844
6.838
6.834
6.833
6.834
6.836
6.840
6.845
6.852
6.859
6.867
6.877
6.886
7.118
7.087
7.059
7.036
7.016
7.000
6.987
6.977
6.970
6.965
6.964
6.965
6.968
6.974
6.982
6.992
7.004
7.018
7.034
-
7.534
7.500
7.472
7.448
7.429
7.413
7.400
7.389
7.380
7.373
7.367
7.361
-
9.464
9.395
9.332
9.276
9.225
9.180
9.139
9.102
9.068
9.038
9.011
8.985
8.962
8.941
8.921
8.900
8.885
8.867
8.850
-
10.317
10.245
10.179
10.118
10.062
10.012
9.966
9.925
9.889
9.856
9.828
9.813
9.782
9.765
9.751
9.739
9.731
9.726
9.724
-
119
9 Annex
9.5 Standard equipment
Immediately upon receipt of the instrument please check that the delivery is
complete. The illustrations in the lists of accessories are not to the same
scale.
9.5.1 pH960 pH Meter
The pH Meter pH960 is supplied with the following accessories:
No.
Order No.
Description
1
PN 3900-096 pH Meter pH960
1
PN 3900-103 101 Magnetic Stirrer
1
PN 3900-100 LL Unitrode Pt1000
comb. pH glass electrode
Pt1000 temp. sensor
El. plug F, T. plug 2mm
1
PN 390-101
1
PN 3900-053 Clamping ring 10 mm
1
PN 3900-102 Support rod
400 mm x 10 mm
1
PN 3900-050 Electrode holder
made of plastic
1
PN 3900-106 Power supply
100-240V, 50-60Hz / 12 V DC
Base plate for pH960
Mains cable:
PN 3900-107 mains cable 2 Pol (C7) – EU (XVI)
PN 3900-108 mains cable 2 Pol (C7) – US (N1/15)
PN 3900-109 mains cable 2 Pol (C7) – GB (BS89/3)
PN 3900-110 mains cable l 2 Pol (C7) –AUS (SAA/2)
120
9 Annex
1
1
Allen key
PN 3900-111 5 mm
PN 3900-112 2 mm
1
350-8110-000 Instructions for use pH Meter pH960
121
9 Annex
9.6 Optional accessories
9.6.1 Various
Order no.
PN 3900-113
PN 3900-114
Description
16 mm x 4 mm
25 mm x 4 mm
Stirring bar
PTFE-coated
PN 3900-040 pH buffer set
50 mL concentrate of each for dilution to 250 mL
pH 4, pH 7, KCl 3 mol/L
PN 3900-041 pH 4
PN 3900-042 pH 7
PN 3900-043 pH 9
pH buffer set
ready-to-use, 3 x 50 mL concentrate of each for dilution to 250 mL
PN 3900-045 pH 4
PN 3900-046 pH 7
PN 3900-047 pH 9
pH buffer solution
ready-to-use, 500 mL of each
PN 3900-048 Electrolyte solution 3 mol/L KCl, 250 mL (for Ag/AgCl reference systems)
9.6.2 Connections
PN 3900-016 RS232/Parallel converter
Connects printers with a parallel interface to pH960-RS 232
PN 3900-017 Cable
Connection cable
pH960-RS 232 —PC (25-pin)
PN 3900-018 3 m
PN 3900-019 5 m
Cable
Connection cable
pH960-RS 232 —PC (9-pin)
PN 3900-020 Cable
Connection cable pH960-RS 232 —
printer (e.g. Citizen iDP 562 RS, Epson
LX 300, HP DeskJet serial)
PN 3900-021 Cable
Connection cable 780/781-RS 232 —
printer (e.g. Custom DP40-S4N,
Seiko DPU-414)
122
9 Annex
9.7 Warranty and conformity
9.7.1 Warranty
The warranty on our products is limited to defects that are traceable to material, construction or manufacturing error which occur within 12 months from
the day of delivery. In this case the defects will be rectified in our workshops
free of charge. Transport costs are to be paid by the customer.
For day and night operation the warranty is limited to 6 months.
Glass breakage in the case of electrodes or other parts is not covered by the
warranty. Checks which are not a result of material or manufac-turing faults
are also charged during the warranty period. For parts from outside manufacturers, insofar as these constitute an appreciable part of our instrument, the
warranty stipulations of the manufacturer in ques-tion apply.
With the regard to the guarantee of accuracy the technical specifica-tions in
the instruction manual are authoritative.
Concerning defects in materials, construction or design as well as the absence of guaranteed features the purchaser has no rights or claims except
those mentioned above.
If damage of the packaging is evident on receipt of a consignment or if the
goods show signs of transport damage after unpacking, the carrier must be
informed immediately and a written damage report demanded. Lack of an official damage report releases Precisa from any liability to pay compensation.
If any instruments and parts have to be returned then the original pack-aging
should be used if at all possible. This applies above all to instru-ments and
electrodes. Before embed-ment in wood shavings or similar material the parts
must be packed in a dustproof package (for instruments the use of a plastic
bag is essen-tial). If open assemblies are included that are sensitive to electromag-netic voltages (e.g. data interfaces, etc.) then these must be returned
in the associated original protective packaging (e.g. conductive protective
bag). (Exception: assemblies with a built-in voltage source belong in nonconductive protective packaging).
For damage which arises as a result of non-compliance with these instructions no warranty responsibility whatsoever will be accepted by Precisa.
9.7.2 EU Declaration of Conformity for pH960 pH Meter
EU Declaration of Conformity
123
9 Annex
The company Metrohm AG, Herisau, Switzerland, certifies herewith, that the following instrument:
pH960 pH Meter
meets the CE mark requirements of EU Directives 89/336/EEC and 73/23/EEC.
Source of specifications:
EN 61326-1
EN 61010-1
Electrical equipment for measurement, control and laboratory use
– EMC requirements
Safety requirements for electrical equipment for measurement,
control and laboratory use
Description of apparatus:
Universal and fully configurable potentiometric measuring instrument for direct
measuring of pH, potential and temperature; continuous display of measured
value on dot-matrix display; connection for measuring electrode, reference electrode and temperature sensor as well as stirrer, serial printer or PC and keyboard
or barcode reader.
Herisau, July 1, 2002
124
Dr. J. Frank
Ch. Buchmann
Leiter Entwicklung
Leiter Produktion und
Beauftragter Qualitätssicherung
9 Annex
9.7.3 Certificate of Conformity and System Validation: pH960 pH Meter
Certificate of Conformity and System Validation
This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to
system validation issued by the manufacturing company.
Name of commodity:
pH960 pH Meter
System software:
Stored in Flash ROMs
Name of manufacturer:
Metrohm Ltd., Herisau, Switzerland
This Metrohm instrument has been built and has undergone final type testing according to the standards:
Electromagnetic compatibility: Emission
IEC 61326-1, EN 55022, IEC 61000-3-2, IEC 61000-3-3
Electromagnetic compatibility: Immunity
IEC 61326-1, IEC 61000-4-2, IEC 61000-4-3, ENV 50204, IEC 61000-4-4,
IEC 61000-4-5, IEC 61000-4-6, IEC 61000-4-11
Safety specifications
IEC 61010-1, UL3101-1
The technical specifications are documented in the Instructions manual.
The system software, stored in programmable Read Only Memories (Flash-ROMs)
has been validated in connection with standard operating procedures in respect to
functionality and performance.
Metrohm Ltd. is holder of the SQS-certificate of the quality system ISO 9001 for
quality assurance in design/development, production, installation and servicing.
Herisau, July 1, 2002
Dr. J. Frank
Ch. Buchmann
Development Manager
Production and
Quality Assurance Manager
Certificate of Conformity and System Validation:
Quality Assurance Manager
125
Index
Index
<
<‘>, <’>.........................26, 27
<-/exp>......................................26
<ABC> ......................................26
<CAL.DATA>.............................24
<CAL> .......................................24
<CLEAR> ..................................27
<CONFIG>................................23
<CONTRAST- > ........................27
<CONTRAST+ >.......................27
<EL.TEST> ................................25
<ENTER> ..................................27
<MEAS/PRINT>...................24, 35
<METHODS> ............................26
<MODE> ...................................24
<ON/OFF> ................................23
<PARAM> .................................23
<QUIT> .....................................24
<RECALL> ................................25
<REPORT>................................25
<SELECT> ................................26
<STIRRER> ...............................26
<STORE> ..................................25
<USER> ....................................24
A
Accessories
Connection...............................9
Standard equipment ............128
Accuracy...................................113
Adapter 4mm/2mm...................128
AD-Converter Test............100
Alkali error .................................119
Ambient temperature ................114
Annex ........................................112
Asymmetry potential .................117
Attention........................................6
Auxiliaries ....................................40
B
barcode reader
Configuration..........................45
Base plate.................................128
baud rate................................45
beep ...........................................42
Buffer recognition .......................53
Buffer set...................................130
Buffer tables..............................124
buffer type
Calibration parameter pH.......53
pH calibration data.................68
C
c.dat.
pH calibration data.................67
Cable PN 3900-120 ....................13
Cable PN 3900-121 ....................13
Cables
Order information .................130
CAL.DATA
pH...........................................66
cal.interval
pH calibration data.................67
cal.table
pH calibration data.................69
Calibrated Reference 2.767.0010
.............................................101
Calibration data
Electrode Id ............................48
Limits pH ................................54
pH...........................................66
calibration interval
calibration parameter pH .......52
Calibration parameters
pH...........................................50
calibration report ...........36
Calibration report ........................76
Cancel.........................................24
CE label ....................................133
Certificate
Conformity............................134
EU Declaration of Conformity
.........................................133
character set
Configuration..........................44
Check the meas. input..............101
Checks..........................................8
Clamping ring .....................11, 128
CONFIG
Description .............................31
Menu structure .....................120
Configuration ..............................31
Menu structure .....................120
Configuration report....................77
Conformity ........................133, 134
Connection
Devices...................................12
Electrodes/Sensors ................14
Printer .....................................12
Stirrer ......................................11
Connection cables
Order information .................130
Connections..................................4
curve
pH calibration data.................70
D
Danger ..........................................6
data bit ..................................45
date
Configuration..........................41
date & time
Report configuration...............33
Delete electrode Id
pH calibration data.................69
delta measurement
Measuring parameter pH .......49
Measuring parameter T..........59
Measuring parameter U .........63
device label .........................42
Diagnosis ....................................99
Dialog language..........................40
Dimensions ...............................114
display ....................................41
drift
Calibration parameter pH.......52
Measuring parameter pH .......48
Measuring parameter T..........58
Measuring parameter U .........62
print criterion ..........................38
Storage criterion .....................39
Drift
Electrode test .......................107
Drift control
pH...........................................49
dU
Electrode test .......................107
E
Editing .........................................29
EL.TEST ....................................104
electr.id
Measuring parameter pH .......48
Measuring parameter T..........58
Measuring parameter U .........62
pH calibration data.................66
Electrical safety .............................7
Electrode holder........................128
electrode id
Report configuration...............33
Electrode out of limits ...............109
Electrode test
Buffers ..................................104
Description ...........................104
Measures..............................109
Messages.............................109
Parameter pH .........................57
Procedure.............................105
Results..................................107
Test criteria ...........................110
electrode type
Electrode test parameter........57
Electrode type
Electrode test tolerances .....108
Electrodes
Connection .............................14
Electrolyte solution....................130
1
Index
Electromagn. compatibility....... 114
EMC.......................................... 114
Emission ................................... 114
EU Declaration of Conformity
pH960 pH Meter .................. 133
Evaluation
pH calibration....................... 116
F
Faults
General .................................. 89
frame ........................................ 87
Front view ..................................... 3
G
Gel electrodes
El. type electrode test ............ 57
General handling rules ................. 7
GLP............................................. 98
Good electrode ........................ 108
Graphics ..................................... 87
grid........................................... 87
H
handshake ............................... 45
Hysteresis
How it functions ..................... 84
Parameter pH......................... 55
Parameter T ........................... 60
Parameter U........................... 64
I
Id1, Id2.................................. 32
immediate
Print criterion .......................... 35
Storage criterion..................... 39
Immunity ................................... 114
Information.................................... 6
Init. of the instrument memory.... 99
Initial configuration ..................... 16
Input assignment........................ 87
Input resistance ........................ 112
Installation............................... 8, 17
Instructions for Use ...................... 5
Instrument description.................. 1
instrument id ...................... 33
Instrument setup........................... 8
Interfaces .................................. 113
Introduction................................... 1
IQ. ............................................... 95
ISO 9100................................... 134
Isothermal intercept point......... 119
K
Key Test................................ 100
keyboard
Configuration ......................... 44
2
Keypad .......................................21
Keys
Functions ...............................23
Illustration.................................3
L
last digit ......................................40
LCD Display Test..............100
LCD off after.......................41
Limit monitoring ..........................83
How it functions .....................84
Limits pH
Parameter pH.........................55
Limits pH(0)
Calibration parameter pH ......54
Limits T
Parameter pH.........................55
Parameter T............................59
Limits U
Parameter U ...........................63
Line feed................................33
Linear regression ......................118
LL Unitrode Pt1000 ...................128
Location ........................................8
Locking .......................................86
M
Magnetic stirrer
Connection.............................11
Mains cable ................................15
Meas. values memory report......79
MEAS/PRINT...............................74
Measured value display..............22
Measured values
Printout...................................35
Measured values memory ..........81
Measuring accuracy .................113
Measuring amplifier check .......101
Measuring interval ....................112
Measuring parameters
param. pH ..............................48
param. T.................................58
param. U ................................62
Measuring point report ...............74
Measuring ranges.....................113
Memory initialization ...................99
Menu display ..............................22
Menu structures........................120
Messages ...................................90
method
Measuring parameter pH.......49
Measuring parameter T..........58
Measuring parameter U .........62
pH calibration data.................66
Report configuration ..............33
Methods
Description.............................46
Management ..........................46
Monitoring...................................43
N
Nernst constant ........................116
Nernst equation ........................116
Netzteil ......................................128
no.of buffers
pH calibration data.................69
Non-aqueous electrodes
El. type electrode test ............57
Notations ......................................6
NTC
Characteristics .....................112
Configuration..........................41
number of buffers
Calibration parameter pH.......52
O
Offset potential ...........54, 112, 116
Electrode test .......................107
offset Uoff state
Calibration parameter pH.......54
ON/OFF ......................................23
Open text editor ..........................26
Operating tutorial ........................17
Operation
Concept..................................22
Key Functions ........................23
Keypad...................................21
Principles................................28
OQ ..............................................95
P
Packaging.....................................8
Paper feed ..................................33
PARAMETER pH .........................48
Parameter report.........................78
PARAMETER T ...........................58
PARAMETER U ...........................62
Parameters
Description .............................46
Menu structure .....................122
parity ......................................45
Parts and controls.........................3
Passing electrode .....................108
Peripheral units
Configuration..........................44
pH buffer set .............................130
pH calibration
Evaluation.............................116
Tutorial....................................18
pH calibration curve..................117
pH calibration data .....................66
pH electrode test ......................104
pH electrodes
Care......................................110
Storage.................................111
pH measurement
Operating tutorial ...................17
Parameters.............................48
pH mode
Parameters.............................48
pH(0)
Index
Evaluation.............................117
pH calibration data.................67
Pictograms....................................6
plot
Print criterion ..........................38
Plot
Adjust size..............................87
Printout ...................................75
Plot parameters
param. pH ..............................56
param. T.................................60
param. U ................................64
poststir pause
Measuring parameter pH.......50
Measuring parameter T..........59
Measuring parameter U .........63
Potential measurement
Parameter...............................62
Power supply ............................113
Precisa buffers............................53
Preselections
Parameter pH.........................56
Parameter T............................60
Parameter U ...........................64
prestir pause
Measuring parameter pH.......50
Measuring parameter T..........59
Measuring parameter U .........63
Principle of the smallest mean
square error..........................118
print crit. ...........................35
Print criterion...............................35
Print measured values ................81
Printer
Configuration..........................44
Connection.............................12
program ....................................42
Pt1000
Configuration..........................41
Q
QM support.................................95
Quality management ..................95
Quality monitoring.......................43
R
RAM Initialization ...........99
RAM Test ................................100
Rear view ......................................4
RECALL ......................................82
reference
Measuring parameter pH.......49
Measuring parameter T..........59
Measuring parameter U .........63
Reference conditions................114
Remote box
Connection...............................4
Remote output
Limit monitoring .....................84
report
Calibration parameter pH.......52
Electrode test parameter........57
Report
Arrangement...........................73
Calibration data ......................76
Configuration....................32, 77
Finishing line ..........................73
Measured values memory......79
Measuring points....................74
Output ....................................71
Overview.................................71
Parameter...............................78
Plot characteristics .................87
Selection.................................71
User method ..........................80
Report header.......................32, 73
Print criterion ..........................36
report id................................33
Report Id .....................................74
Report identification....................74
req.ident
Parameter T............................60
Parameter U ...........................64
req.ident.
Parameter pH .........................56
reset cal
pH calibration data.................69
Resolution .................................113
Response time
Electrode test .......................107
RS232 settings............................45
RS232/Parallel converter
Accessories..........................130
Usage .....................................13
Rubber feet .................................10
run number .................................40
S
Safety information .........................7
Safety specifications .................114
Sample identification
Parameter pH .........................56
Parameter T............................60
Parameter U ...........................64
Save
Measured values....................81
Method ...................................46
Sensors
Connection .............................14
service
Monitoring ..............................43
Setup...........................................86
Show measured values ..............82
signature
Configuration..........................33
Signature
Report.....................................73
slope
pH calibration data.................66
Slope
Electrode test .......................107
pH calibration evaluation .....117
Slope limits
Calibration parameter pH.......54
Stand base....................................9
Standard electrodes
El. type electrode test.............57
Standard equipment .................128
stir time
Measuring parameter pH .......50
Measuring parameter T..........59
Measuring parameter U .........63
stirrer
Measuring parameter pH .......49
Measuring parameter T..........59
Measuring parameter U .........63
Stirrer
Connection .............................11
Electrode test .......................104
Stirring bar ................................130
stirring rate
Measuring parameter pH .......50
Measuring parameter T..........59
Measuring parameter U .........63
Stirring sequence
Measuring parameter pH .......50
Measuring parameter T..........59
Measuring parameter U .........63
stop bit ..................................45
stop time
Print criterion ..........................37
Storage criterion .....................39
STORE ..................................39, 81
store crit..............................39
Stored buffer series...................124
Storing measured values............39
Streaming potential
Electrode test .......................107
Support rod...............................128
Switch on ....................................15
System test
Description .............................97
Report.....................................97
system test report
Monitoring ..............................44
T
T mode
Parameters .............................58
Technical data ..........................112
temp.sensor
Configuration..........................41
pH calibration data.................67
temp.unit................................42
temperature
Calibration parameter pH.......50
Electrode test parameter........57
Measuring parameter pH .......49
pH calibration data.................67
Temperature
Electrode test .......................105
Temperature compensation .....119
Temperature measurement
Parameters .............................58
Text editor ...................................30
time
Configuration..........................41
Print criterion ..........................36
Storage criterion .....................39
time counter
3
Index
Validation ............................... 43
time interval
Print criterion .......................... 36
Storage criterion..................... 39
Validation ............................... 43
time zone ............................... 41
TIP................................................. 6
Transport ...................................... 8
Troubleshooting.......................... 88
Parameters.............................62
U/pH curve................................116
Unitrode ....................................128
Uoff
Electrode test .......................107
USER ..........................................24
User method report ....................80
U
validation
Monitoring ..............................43
Validation ....................................97
U mode
4
V
Validation documentation...........95
variance
pH calibration data.................67
Variance
pH calibration evaluation .....118
Various functions ........................65
Version number ..........................42
Very good electrode .................108
W
Warning.........................................6
Warranty....................................132
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