Metrohm 730 User manual

CH-9101 Herisau/Switzerland
Tel. [phone]
Fax [phone]
E-Mail [email protected]
Internet http://www.metrohm.ch
730 Sample Changer
and 759 Swing Head
Program version 5.730.0013
8.730.1103
98.2 sn

Table of Contents
Page
1 OVERVIEW ___________________________________________ 1
1.1 Application Range ________________________________ 1
1.2 Scope on Applications ____________________________ 1
1.3 Instrument Description ____________________________ 3
1.3.1 Side View ......................................................................3
1.3.2 Rear View ......................................................................4
1.3.3 Sensors .........................................................................5
1.3.4 The Sample Changer Models .......................................6
1.3.5 The Swing Head ............................................................6
2INSTALLATION ________________________________________ 7
2.1 Setting up the Instrument __________________________ 7
2.2 Power Supply ____________________________________ 7
2.3 Safety Considerations _____________________________ 9
2.4 Arranging the Accessories ________________________ 10
2.4.1 Connecting the Keyboard ............................................10
2.4.2 Setting up the Rinsing Equipment ...............................10
2.4.3 Tubing Fixation ............................................................12
2.4.4 Magnetic Stirrers .........................................................12
2.4.5 Sample Racks .............................................................12
2.4.6 Mounting and Setting up the Titration Heads ..............13
2.5 Integration _____________________________________ 14
2.5.1 Remote Connections ...................................................15
2.5.2 External Bus Connections ...........................................23
2.5.3 Serial Connections (RS232).........................................24
2.5.4 Connecting a Printer ...................................................25
3 INTRODUCTION _______________________________________ 27
3.1 Tutorial ________________________________________ 27
3.2 Configuration ___________________________________ 35
3.2.1 Basic Settings .............................................................35
3.2.2 Rack Definition ............................................................37
3.2.3 Dosing Units ................................................................39
3.2.4 RS232 Interface ..........................................................40
3.2.5 Locking Keyboard Functions .......................................40
3.3 Swing Head _____________________________________ 42
3.3.1 Prerequisites ...............................................................42
3.3.2 Installing the Swing Head ............................................42
3.3.3 Accessories for the Titration Head ..............................44
3.4 Manual Operation _______________________________ 46
3.5 Methods and Sequences __________________________ 49
3.5.1 Composition of a Method ............................................50
3.5.2 LEARN Mode and TRACE Function ...........................51
3.5.3 Process Control ..........................................................52
3.5.4 POWERUP Method .....................................................52
3.6 User Methods ___________________________________ 53
4DETAILED DESCRIPTION ________________________________ 59
4.1 The Display _____________________________________ 59
4.2 The Keyboard ___________________________________ 60
4.2.1 Individual Key Functions .............................................61
4.2.2 Data Entry ...................................................................78
4.2.3 Text Entry ....................................................................79

Table of Contents
Page
4.3 Menu Organization _______________________________ 81
4.3.1 Configuration ..........................................................82
4.3.2 Parameters ............................................................87
4.3.3 User Defined Methods ............................................93
4.4 Changer Commands ______________________________ 94
4.5 Sample Racks __________________________________ 104
4.6 Dosimats and Dosinos ___________________________ 109
4.7 Pipetting with the Swing Head ____________________ 114
4.7.1 Setting up the System ...........................................114
4.7.2 Example Pipetting Method .....................................115
4.8 Remote Interface ________________________________ 119
4.9 Operation via RS 232 Interface ____________________ 125
4.9.1 General Rules .......................................................125
4.9.2 Calling up Objects.................................................126
4.9.3 Trigger .................................................................127
4.9.4 States and Error Messages ...................................127
4.9.5 Error Messages.....................................................128
4.10 Remote Control Commands ______________________ 130
4.10.1 Overview..............................................................130
4.10.2 Description of the Remote Control Commands ......139
4.11 Properties of the RS 232 Interface_________________ 155
4.11.1 Data Transfer Protocol .........................................155
4.11.2 Handshake...........................................................155
4.11.3 Pin Assignment ....................................................159
4.11.4 What to do if Data Transfer fails............................160
5 APPENDIX__________________________________________ 161
5.1 Error Messages _________________________________ 161
5.2 Technical Specifications _________________________ 163
5.2.1 730 Sample Changer ............................................163
5.2.2 759 Swing Head ...................................................165
5.3 Servicing and Maintenance _______________________ 166
5.3.1 Servicing...............................................................166
5.3.2 Maintenance / Attendance......................................166
5.4 Diagnosis ______________________________________ 167
5.4.1 General Informations ............................................167
5.4.2 Preparing the Instrument .......................................168
5.4.3 Working Memory (RAM) .......................................169
5.4.4 Display ................................................................169
5.4.5 Keyboard .............................................................170
5.4.6 Remote Interface ..................................................171
5.4.7 RS 232 Interface ..................................................172
5.4.8 External Bus Interface ..........................................172
5.4.9 Beeper .................................................................173
5.4.10 Rack Code Recognition ........................................173
5.5 Initialize data memory____________________________ 175
5.6 Validation / GLP ________________________________ 177
5.7 Warranty and Conformity ________________________ 178
5.7.1 Warranty ..............................................................178
5.7.2 Certificate of Conformity and System Validation
for the 730 Sample Changer ...........................179
5.7.3 Certificate of Conformity and System Validation
for the 759 Swing Head ..................................181
5.8 Accessories ____________________________________ 183
5.9 Index __________________________________________ 189
Quick Reference _______________________________________

1.1 Application Range
730 Sample Changer, Overview 1
1 Overview
1.1 Application Range
The Metrohm 730 Sample Changer is an instrument for numerous
applications. It was specially developed for the industrial or ana-
lytical laboratory and therefore covers a wide spectrum of applica-
tions. It provides indispensable support when processing a large
sample series in the entire range of titrations, for various meas-
urement jobs, or for dosing purposes.
Due to the well-developed communication interfaces (parallel re-
mote control and serial RS 232) it can not only communicate with
the large palette of Metrohm titration and dosing instruments; it
can also control or be controlled by any instrument that has a suit-
able communication interface. These capabilities predestine it for
all conceivable automatization jobs in a modern laboratory, even in
conjunction with highly integrated laboratory data systems.
1.2 Scope on Applications
In spite of the extensive range of commands and configuration
possibilities, the mode of operation is uncomplicated thanks to the
ability for managing user-defined methods, making it suitable for
routine use.
The user methods provided are industry-oriented and may be
used “as is” for routine assignments. After a short training period
the user can modify them for his own purposes and store them in
the instrument. The 730 Sample Changer can therefore be used
for challenging special applications as well as for routine jobs.

1.2 Scope on Applications
730 Sample Changer, Overview
2
The sequences for the processing of each sample are freely de-
finable within broad boundaries. The same is true for the start and
end sequences that are executed once either before or at the end
of a sample series. This is advantageous specially for titrations.
The electrode can be conditioned prior to use or subjected to a
special rinse procedure at any time.
With the help of the LEARN mode, which is provided for creating
process methods, a method can be created easily.
Standard interchangeable racks are provided for various beaker
sizes. Freely-definable "special beaker" positions can be defined
for every rack. They define a rack position for rinse or conditioning
beakers that can then be selected in any sub-sequence.
Position tables which describe user-defined special racks may be
downloaded via RS232 interface with the aid of a suitable PC
software.
In order to increase the number of samples that can be treated,
the 759 Swing Head can be installed. This drive is installed in-
stead of the normal titration head and is obtainable in two ver-
sions: either with a titration head for the direct titration in the sam-
ple vessels or with a transfer head, with the help of which the
samples can be transferred from test tubes into a central titration
vessel.

1.3 Instrument Description
730 Sample Changer, Overview 3
1.3 Instrument Description
1.3.1 Side View
Safety note:
Never operate the 730 Sample Changer without splash protection
and plug cover being mounted.
The plug cover prevents any contamination of the connectors,
caused by spilled solvents or chemicals.
Splash protection
Plug cover
Rack Lift Pump
Guide chain
Tower
Connectors
Stirrer rail
Distribution
head
Valve

1.3 Instrument Description
730 Sample Changer, Overview
4
The Connectors (side view):
Remote
Control
1
2
3 4
WARNING - Fire Hazard -
For continued protection replace only
with the same type and rating of fuse
The remote socket serves the connection of Metrohm- or other
measuring instruments that communicate via a serial cable.
1.3.2 Rear View
Made by Metrohm Herisau Switzerland
RS 232 Keyboard
Type 1.730._
Address
External Bus
0020/01 113
Remote
socket
Stirrer sockets
Power switch
Power socket
Guide chain
Fuse holder
Mounting screw
for
Splash protection
Pump 1
Pump 2
Valves
Plug cover
Connectors
Distribution head

1.3 Instrument Description
730 Sample Changer, Overview 5
The Connectors (rear):
Made by Metrohm Herisau
Switzerland
RS 232 Keyboard
Type 1.730._
Address
External Bus 0120/02 187
The External Bus address selector must be set to 0 (zero).
1.3.3 Sensors
Beaker test
Front view
Each tower of the 730 Sample
Changer is equipped with a
beaker indicator to detect the
presence of a beaker in front
of the particular tower. This
infrared sensor detects many
different materials, if any ob-
ject is placed in correct posi-
tion. This beaker test is car-
ried out after each MOVE op-
eration.
Magnetic rack code indicator
The magnetic sensor to detect
the individual rack codes is
mounted below the sample
changer's turntable.
The magnetic binary code of the
racks can only be read, if the
rack is in initial position and
therefore the magnet holder is
in accurate position right above
the rack code indicator.
For this reason the 730 Sample
Changer should be initialized
right after every rack change
by pressing the <RESET> key
or <ENDSEQ> followed by
<ENTER>.
Splash protection
Beaker indicator
Rack
Magnetic indicator
Manufacturing number
Magnet holder
External Bus
socket External Bus
address selector
Serial
RS 232 interface Keyboard
connector

1.3 Instrument Description
730 Sample Changer, Overview
6
11.3.3.4.4 The Sample Changer Models
Model 2.730.0010 Model 2.730.0020 Model 2.730.0030
1 tower, 1 pump 1 tower, 2 pumps 1 tower, no pumps
2 stirrer connections 2 stirrer connections 2 stirrer connections
Model 2.730.0110 Model 2.730.0120 Model 2.730.0130
2 towers, 2 pumps 2 towers, 4 pumps 2 towers, no pumps
4 stirrer connections 4 stirrer connections 4 stirrer connections
11.3.3.5.5 The Swing Head
In order to increase the number of samples, the 759 Swing Head
with a titration head (2.759.0020) or a transfer head (2.759.0010)
can be installed in place of a normal titration head. In this way the
titration head can be moved very accurately to the individual ves-
sels located in several rows on the sample rack. You will find a
more detailed description in chapter 7 "Swing Head", page 42.
Tower 1 Tower 2 Tower 1 Tower 2 Tower 1 Tower 2

2.1 Setting up the Instrument
730 Sample Changer, Installation 7
2 Installation
2.1 Setting up the Instrument
Packaging
The 730 Sample Changer is supplied with the accessories in
separate special packages designed to ensure maximum protec-
tion. These contain shock-absorbing foam linings. As only these
special packages guarantee damage-free transport of the instru-
ment, it is essential you store them in a safe place.
Control
Immediately following delivery, check that the consignment is
complete and undamaged (compare with delivery note and acces-
sories list in the Instructions for Use, page 183). In case of dam-
age see "Warranty", page 178.
Setting up
The 730 Sample Changer is a rugged instrument and may be
used in rough environments such as laboratories and manufac-
turing plants. It must not be exposed to a corrosive atmosphere.
If the sample changer is operated in a rough environment, regular
maintenance is strongly recommended.
2.2 Power Supply
Follow these instructions to connect the 730 Sample Changer to
the power supply. Ensure that the instrument is never operated
with incorrect voltage ratings and/or with fuses of an incorrect rat-
ing, otherwise there is a fire hazard!
Setting the instrument supply voltage
Before switching on the Sample Changer for the first time, check
that the line voltage set on the instrument (see next page)
matches the local power supply voltage. If this is not the case,
change the voltage setting as follows:

2.2 Power Supply
730 Sample Changer, Installation
8
• Disconnect line cable
Unplug the 730 Sample Changer.
• Remove fuse holder
Using a screw driver, loosen the fuse holder and pull it out.
• Checking and replacing fuse
Carefully remove the built-in fuse and check its specifications.
(The position of the fuse in the fuse holder is marked by the
white arrow printed next to the supply voltage):
100……120 V 0.5 A (slow) ord. no. U.600.0014
220……240 V 0.25 A (slow) ord. no. U.600.0011
• Replace fuse
Replace fuse if necessary and reinsert it in the fuse holder.
• Insert the fuse holder
Insert the fuse holder according to the appropriate supply volt-
age. The white arrow besides the desired voltage has to point
towards the white block mark printed on the fuse holder's panel
(see below).
100 – 120 V
220 – 240 V
Power switch
Power plug Fuse holder

2.3 Safety Considerations
730 Sample Changer, Installation 9
2.3 Safety Considerations
If failure or malfunctioning occurs during operation of the 730
Sample Changer, it is recommended to first search for the cause
with the help of the diagnostic functions (see Instructions for Use,
page 167). If this is of no help in rectifying the disorder or the
cause of the malfunction cannot be identified, the Metrohm Serv-
ice Department should be consulted.
If opening the instrument is unavoidable, the following safety pre-
cautions are to be strictly adhered to:
Before opening the instrument disconnect it from all electri-
cal sources. Make sure that the power plug has been pulled
out.
Only in exceptional cases should the instrument be opened while it
is switched on. Because parts that conduct current are exposed in
this case, this should only be undertaken by an expert who is ac-
quainted with the associated dangers.
Electronic components are sensitive to static electricity and can be
destroyed by discharge. Before touching any components inside
the instrument, both the person and his tools should be grounded
by grasping a grounded object (for example: a metallic part of the
casing of the instrument or a radiator) in order to eliminate any
static electricity.
When peripheral instruments are connected to the 730 Sample
Changer, the sample changer and the instruments to be con-
nected have to be switched off, otherwise all instruments could
suffer damage.
If it becomes apparent that the instrument can no longer be oper-
ated safely, it must be put out of operation.

2.4 Arranging the Accessories
730 Sample Changer, Installation
10
2.4 Arranging the Accessories
2.4.1 Connecting the Keyboard
730
The keyboard is to be con-
nected to the keyboard socket
on the rear side of the sample
changer. To disconnect press
the plug together slightly on
both sides.
2.4.2 Setting up the Rinsing Equipment
To mount the PTFE tubings to the pump inlets or outlets enlarge it
carefully using a pen or another appropriate tool. A piece of sand
paper facilitates grasping of the tubing.
The arrangement of the tubing depends on the rinsing equipment.
Rotating nozzle
Using a changer model with one pump per tower only, the rotating
nozzle (6.2740.000) is recommended for rinsing. The Teflon tubing
is then directly connected to the rinsing pump (pump 1). The dis-
tribution head may be dismounted in this case.
Place the rotating nozzle vertically in the titration head with the aid
of a SGJ14/12 mm sleeve.

2.4 Arranging the Accessories
730 Sample Changer, Installation 11
Spray nozzles
When using a changer model with two pumps per tower, spray
nozzles (6.2740.020) may be used in combination with an aspira-
tion tip M8 (6.1543.170). Insert the spray nozzles into the sloped
borings of the titration head. Use Teflon tubings to connect them
to the distribution head. Each of the four outlets of the distribution
head must be plugged. Plug unused outlets with an M6 thread
stopper (6.1446.040) to avoid splashing of liquid during rinsing.
Fix the tubings in the guide chain. Chain links may be removed if
necessary (see below).
Insert the aspiration tip vertically into a boring (SGJ9) of the Macro
Titration Head. The Micro Titration Head offers also a vertical bor-
ing for the placement of the aspiration tip. Connect the tip with the
Teflon 4/6 tubing (6.1805.510) and a screw connector 4/6 mm
(6.1820.030) to pump 2 (valve marked with 'ê'). During the rinsing
procedure, first the sample is sucked off then the electrode is
rinsed in the empty vessel.
The pump heads of the diaphragm pump, the fittings and the cou-
pling rings are made of PVDF. PVDF is resistant to many chemi-
cals. Acetone, acetanhydride or dimethylformamide (DMF) should
not be used. The diaphragm, and the inner parts of the valves
consist of PTFE and are resistant to most chemicals.
If your samples contain solids (e.g. silver chloride) or sticking sub-
stances, you should use the 772 Peristaltic Pump Unit in combina-
tion with the 731 Relay Box instead of the diaphragm pump inte-
grated into the changer.
The PE canisters (6.1621.000) are suitable for aqueous solutions.

2.4 Arranging the Accessories
730 Sample Changer, Installation
12
2.4.3 Tubing Fixation
In order to fix the tubing in
the guide chain any chain link
may be opened with a screw
driver or another appropriate
tool.
2.4.4 Magnetic Stirrers
Magnetic stirrers 2.741.0010
may be placed in any
position on the stirrer rail
beneath the rack.
2.4.5 Sample Racks
After placing the rack on the
turntable, the sample
changer must be initialized
by pressing the <RESET>
key to enable the safe
reading of the magnetic rack
code.
This can only be done if rack
position 1 is directed to
tower 1.
Rack
Stirrer rail
Magnet holder
Magnetic sensor

2.4 Arranging the Accessories
730 Sample Changer, Installation 13
2.4.6 Mounting and Setting up the Titration Heads
Macro Titration head
6.1458.010 Micro Titration head 6.1458.020
Mounting screws
Aspiration tip M8
(also for Macro Titration head )
6.1543.170
Electrode
Rotating nozzle
6.2740.000
Burette tip
Rod stirrer
2.722.0020
M6 Spray nozzles
(also for Macro Titration head)
6.2740.020
SGJ14 sleeve
6.1236.020
M8 Thread stopper
4.658.0180
SGJ9 Guide sleeve
6.2709.070
Stirrer propeller
6.1909.020
Note on Macro Titration head
The arrow sign marks the slightly sloped SGJ boring, which enables to center a rod
stirrer or an electrode in a narrow titration vessel.
Use only the designated
Micro electrodes with the
Micro Titration head, see
accessory list, page 183.

2.5 Integration
730 Sample Changer, Installation
14
2.5 Integration
The 730 Automation System
729
ExternalBus
RS232 Remote
Dosimat
pH-Meter /
Conduktometer
Titrino Family
Titro-
processors
Titroprocessor
Dosino 700 Dosimat 685
PC Software
Printer
TiNet 2.2
730 Sample Changer
665
725
691
692
712
713
718
719
720
736
751
672
678
682
686
670
DosimatInterface729
Seiko
Citizen
Epson
HP
IBM
…
other
instruments
730
758
702
716
Liquino 711
Swing Head 759
Cables
Connecting peripheral instruments to the 730 Sample Changer re-
quires Metrohm cables. Otherwise a safe data transmission may
not be guaranteed.
Remark:
Metrohm cables are labeled with the type of the instrument which
they may be connected with and optionally with the particular
socket. Mind the cable ends.
For example:
Titrino B
692 /712 /713
All instruments have to be switched off, before they are con-
nected. Otherwise the instruments could suffer from damage.

2.5 Integration
730 Sample Changer, Installation 15
2.5.1 Remote Connections
730 Sample Changer — Titrino
with standard cable
730
B
ATitrino
C
D
Remote control commands:
CTL:Rm : START device1 starts Titrino
CTL:Rm : *************1 "
Scan commands:
SCN:Rm : end1 awaits end of titration
SCN:Rm : ****1*** "
SCN:Rm : ready1 awaits readiness of Titrino
SCN:Rm : *******1 "
730 Sample Changer — 691 pH-Meter
730 691
Cable 6.2141.020
Cable 6.2141.060

2.5 Integration
730 Sample Changer, Installation
16
Remote control commands:
CTL:Rm : START device1 starts measuring instrument
CTL:Rm : *************1 "
CTL:Rm : METER mode pH change mode to pH measurement
CTL:Rm : *********0001* "
CTL:Rm : METER mode T change mode to temp. measurement
CTL:Rm : *********0010* "
CTL:Rm : METER mode U change mode to mV measurement
CTL:Rm : *********0011* "
Scan commands:
SCN:Rm : End1 awaits end of measurement
SCN:Rm : ****1*** "
730 Sample Changer — pH- / Ion- / Conductometer
(692/712/713)
692
712
713
730
Remote control commands:
CTL:Rm : START device1 starts measuring instrument
CTL:Rm : *************1 "
CTL:Rm : METER mode pH change mode to pH measurement
CTL:Rm : *********0001* " (not appl. with 712)
CTL:Rm : METER mode T change mode temp. measurement
CTL:Rm : *********0010* " (not appl. with 712)
CTL:Rm : METER mode U change mode to mV measurement
CTL:Rm : *********0011* " (not appl. with 712)
CTL:Rm : METER mode I change mode to Ipol (mV meas.)
CTL:Rm : *********0100* " (not appl. with 712)
CTL:Rm : METER mode C change mode to conc measurement
CTL:Rm : *********1000* " (only appl. with 692)
CTL:Rm : METER cal pH change mode to pH calibration
CTL:Rm : *********0101* " (not appl. with 712)
CTL:Rm : METER cal C change mode to conc calibration
CTL:Rm : *********1001* " (only appl. with 692)
CTL:Rm : METER enter simulates <ENTER> key
CTL:Rm : *********1111* " (not appl. with 712)
Scan commands:
SCN:Rm : end1 awaits end of determination
SCN:Rm : ****1*** "
Cable 6.2141.020

2.5 Integration
730 Sample Changer, Installation 17
730 Sample Changer — 713 / 692 pH/Ionmeter — 665 Dosimat
for automatic calibration including standard addition.
730 692
713 B
A665
C
D
The 692 pH/Ion Meter takes control of stirrer 1 connected to the
730 Sample Changer.
Remote control commands:
The same commands are applicable as above.
Scan commands:
The same commands are applicable as above, but also:
SCN:Rm : endmeter awaits end pulses from 692 Ion Meter
SCN:Rm : ***11*** "
730 Sample Changer — 2 x Titrino
730
B
ATitrino
C
D
B
ATitrino
C
D
device 2
device 1
Cable 6.2141.030
Cable 6.2141.070