Metrohm 774 User Manual
CH-9101 Herisau/Switzerland
Tel. +41 71 353 85 85
Fax +41 71 353 89 01
E-Mail sales@metrohm.ch
Internet http://www.metrohm.ch
774 Oven Sample Processor
Instructions for use
Program version 5.774.0010
8.774.1043
2005.07 dm
Table of contents
Page
1 Overview 1
1.1 Application range___________________________________________ 1
1.2 Application possibilities_____________________________________ 1
1.3 Instrument description ______________________________________ 3
1.3.1 Oblique view from the right-hand side ......................................... 3
1.3.2 Oblique view from left-hand side.................................................. 4
1.3.3 Rear view....................................................................................... 5
1.3.4 The socket strip (rear panel):........................................................ 5
1.3.5 Guide head ................................................................................... 6
1.3.6 Sample rack.................................................................................. 6
1.3.7 Sample vials.................................................................................. 7
2 Installation 8
2.1 Setting up the instrument____________________________________ 8
2.2 Power supply ______________________________________________ 8
2.3 Safety considerations ______________________________________ 10
2.4 Arranging the accessories__________________________________ 11
2.4.1 Connecting the keyboard ........................................................... 11
2.4.2 Equipping the guide head ..........................................................12
2.4.3 Adjusting the sample rack .......................................................... 12
2.4.4 Adjusting the needle position .....................................................13
2.4.5 Installation of the tubing system and the drying flask................ 14
2.4.6 Installation of the measuring cell ................................................ 15
2.5 Integration ________________________________________________ 15
2.5.1 Remote connections................................................................... 16
2.5.2 External bus connections ...........................................................19
2.5.3 Serial connection (RS232) .......................................................... 20
2.5.4 Connecting a printer ................................................................... 21
3 Introduction 23
3.1 Configuration _____________________________________________ 23
3.1.1 Basic settings ............................................................................. 23
3.1.2 Oven settings.............................................................................. 24
3.1.3 Rack definitions .......................................................................... 25
3.1.4 Dosing units ................................................................................ 26
3.1.5 RS232 interface........................................................................... 27
3.1.6 Lock keyboard functions ............................................................28
3.2 Manual operation __________________________________________ 30
3.3 Methods and Sequences ___________________________________ 33
3.3.1 Designing a method ................................................................... 33
3.3.2 LEARN mode and TRACE function ............................................ 34
3.3.3 Process control........................................................................... 35
3.3.4 POWER-UP methods.................................................................. 36
4 Oven control and gas flow 37
4.1 Oven control ______________________________________________ 37
4.2 Gas flow __________________________________________________ 38
4.3 KF Moisture determination _________________________________ 40
Table of contents
5 Detailed description 43
5.1 The display ________________________________________________43
5.2 The keyboard ______________________________________________44
5.3 Menu organization _________________________________________62
5.4 Command reference________________________________________76
5.5 Printing reports ____________________________________________ 85
5.6 Sample racks ______________________________________________89
5.7 Dosimats and Dosinos______________________________________92
5.8 Remote Interface ___________________________________________97
5.9 Operation via RS232 Interface______________________________101
5.10 The remote control tree ___________________________________106
5.11 Description of the remote control commands _______________116
5.12 Properties of the RS232 Interface __________________________131
Page
5.2.1 Individual key functions .............................................................. 45
5.2.2 Data entry ................................................................................... 59
5.2.3 Text Entry .................................................................................... 60
5.3.1 Configuration .............................................................................. 63
5.3.2 Parameters ................................................................................. 68
5.3.3 User Defined Methods ............................................................... 75
5.5.1 Automatic reports ....................................................................... 88
5.5.2 Manual reports............................................................................ 88
5.9.1 General rules ............................................................................ 101
5.9.2 Calling up Objects ................................................................... 102
5.9.3 Triggers..................................................................................... 103
5.9.4 Status and Error Messages...................................................... 103
5.9.5 Error Messages, Errors............................................................. 104
5.10.1 Overview ................................................................................. 106
5.10.2 &Mode .................................................................................... 106
5.10.3 &Config................................................................................... 108
5.10.4 &Info ....................................................................................... 109
5.10.5 &Setup .................................................................................... 112
5.10.6 &UserMeth.............................................................................. 113
5.10.7 &Assembly.............................................................................. 113
5.10.8 &Diagnose.............................................................................. 115
5.11.1 &Mode … ............................................................................... 116
5.11.2 &Config … .............................................................................. 119
5.11.3 &Info …................................................................................... 122
5.11.4 &Setup … ............................................................................... 125
5.11.5 &UserMeth …......................................................................... 127
5.11.6 &Assembly …......................................................................... 128
5.11.7 &Diagnosis … ........................................................................ 130
5.12.1 Data Transfer Protocol ........................................................... 131
5.12.2 Handshake ............................................................................. 131
5.12.3 Pin Assignment....................................................................... 135
5.12.4 What to do if Data Transfer fails? ........................................... 136
Table of contents
Page
6 Appendix 137
6.1 Error messages __________________________________________ 137
6.2 Technical data____________________________________________ 140
6.3 Maintenance and servicing ________________________________ 142
6.3.1 Maintenance / service............................................................... 142
6.3.2 Servicing / care ......................................................................... 142
6.4 Diagnosis ________________________________________________ 143
6.4.1 General ..................................................................................... 143
6.4.2 Preparing the instrument ..........................................................144
6.4.3 Main memory (RAM)................................................................. 145
6.4.4 Display ......................................................................................145
6.4.5 Keypad...................................................................................... 146
6.4.6 Remote interface....................................................................... 146
6.4.7 RS232 interface......................................................................... 147
6.4.8 External bus interface ...............................................................147
6.4.9 Beeper....................................................................................... 148
6.4.10 Rack code recognition............................................................ 148
6.5 Initialise data memory_____________________________________ 149
6.6 Validation / GLP __________________________________________ 152
6.7 Warranty and Conformity__________________________________ 154
6.7.1 Warranty.................................................................................... 154
6.7.2 EU Declaration of Conformity ................................................... 155
6.7.3 Certificate of Conformity and System Validation...................... 156
6.8 Accessories______________________________________________ 157
7 Index 159
1.1 Application range
1 Overview
1.1 Application range
The Metrohm 774 Oven Sample Processor is a very versatile instrument. It
has been specially designed for laboratory use and can be used for a wide
range of applications. It provides an essential service when large numbers
of samples have to be processed in which the samples require to be
heated and/or whenever it is necessary to remove moisture or organic solvents from solids or liquids by the application of heat.
The construction of the 774 Oven Sample Processor has been principally
based on the determination of moisture by the oven method. The sample
heated in the oven block releases its moisture as water vapor which is
transferred to a measuring cell in a stream of gas. The moisture determination in the cell can be carried out either coulometrically or volumetrically according to Karl Fischer.
This method is becoming increasingly popular wherever moisture determinations have to be carried out in matrices which interfere with the moisture
determination process or which release their moisture only with great difficulty.
Its comprehensive range of communications possibilities means that it
cannot just work together with the wide range of Metrohm titrators, meters
and dosing instruments via its parallel remote interface and its serial RS232
interface, but that it can also control or be controlled by any instrument
which is equipped with a suitable communications interface. These abilities
mean that it is predestined for automation tasks in a modern laboratory,
even within highly integrated laboratory data systems.
1.2 Application possibilities
Despite its comprehensive range of commands and numerous configuration possibilities the 774 Oven Sample Processor, with its capability of
managing operator-defined methods, offers an uncomplicated operation
system which is suitable for routine use.
The standard methods for routine tasks which we supply together with the
instrument can be used without any further ado. After a short familiarization
period the operators can alter them to suit their own requirements and store
them in the instrument. In this way the 774 Oven Sample Processor can
774 Oven Sample Processor, Instructions for use
1
1 Overview
also be used for demanding special applications as well as for routine
tasks.
The operating sequences for processing individual samples can be freely
defined within wide limits. The same applies to the start and final sequences, which always need to be carried out once before the start and
once at the end of a sample series.
A learning mode is provided for the creation of operating sequences; with
its help command parameters can be set manually.
The standard sample rack offers place for 36 sample vials (22 mm x 38
mm). Freely definable "special beaker" positions can also be defined. These
are used for positioning conditioning beakers, which can be selected in
each part-sequence, on the rack.
2
774 Oven Sample Processor, Instructions for use
1.3 Instrument description
A
1.3 Instrument description
1.3.1 Oblique view from the right-hand side
equipped with Coulometer cell
Gas supply
Protective cover
Sample rack with 36
places (including conditioning position)
Lift
Guide rod
(adjust-
Guide head
Double
hollow needle
ir inlet filter
Connection for
outlet heater
Outlet heater /
transfer hose
Support rod
Coulometer cell
with generatorand indicator
electrode
Magnetic stirrer
The socket strip:
Mains switch
Fuse holder
Mains connection
Oven with
protective jacket
Plug cover
Remote
interface
774 Oven Sample Processor, Instructions for use
3
1 Overview
j
1.3.2 Oblique view from left-hand side
with protective cover in position
Flow regulator
Protective cover
Gas supply
Inert gas
Drying flask
connections
Holder for
drying flask
Drying flask with
molecular sieve
inlet
Sample rack
with grip
Oven with
protective
acket
Safety information:
The protective cover and the plug cover have to be in position for
safety reasons.
The plug cover prevent spilt solvents or chemicals from adversely
affecting the connections and interfaces.
4
774 Oven Sample Processor, Instructions for use
1.3 Instrument description
p
/
1.3.3 Rear view
Air inlet filter
Outlet heater
transfer tube
Plug
cover
Gas supply
Flow regulator
Inert gas inlet
Sample rack
Drying flask
External Bus
Address
1.3.4 The socket strip (rear panel):
External Bus
Address
External bus
connection
External bus
address
selector
The 'External Bus' address must be set to 0 (zero).
0000/ 00 00
Type 1.774._
RS 232 Keyboard
Made by Met rohm Herisa u Switzerl and
Serial number
Serial
RS 232 interface
Rear socket
stri
Type 1.774. _
RS 232
Made by Metrohm Heri sau Switz erland
0000/ 00 00
Keyboard
Keyboard
connection
774 Oven Sample Processor, Instructions for use
5
1 Overview
(
1.3.5 Guide head
Gas supply
(gas inlet)
Guide rod
(adjustable)
Infrared
sensors
Heated transfer hose
(outlet heating)
Needle adapter
made of PEEK
Hollow needle with
Luer connection
exhaust)
Hollow needle
(injection needle)
The tower of the 774 Oven Sample
Processor is equipped with infrared
beaker sensors which detect the
presence of a vial in front of the
tower. This "beaker test" is carried
out after every MOVE command.
1.3.6 Sample rack
Special position 1 (for conditioning vial)
.
d
on
C
.
os
P
Grip
Openings for
guide bolts
Warning!
If sample vials on the racks have just been processed
they could have a temperature above 200°C!
The removable sample rack offers
space for 35 sample vials and a conditioning vessel. A snap-in mechanism
ensures that the rack base is blocked
when the rack is removed so that no
sample vials can fall out. When the
rack is replaced this block is removed
so that the upper part of the rack with
the sample vials can be rotated.
The rack can only be exchanged in the
base position (recess in front of the
tower). The sample rack is moved to
the base position by pressing the
<RACK> key.
When replacing the rack take care that
it is positioned correctly. The guide
bolts of the turntable must be located
in the openings provided for them in
the sample rack. The recess of the
rack must surround the oven block.
6
774 Oven Sample Processor, Instructions for use
1.3 Instrument description
When the sample rack is positioned the rod magnets on the base of the
rack are read in automatically. The arrangement of the magnets defines the
rack code, which is allocated to an internal position table with whose help
the 774 Oven Sample Processor recognizes the arrangement of the vial positions on the rack.
The above arrangement corresponds to the magnet code 000001.
1.3.7 Sample vials
The sample rack (order no. 6.2041.700) is intended for use with sample vials (order. no. 6.2419.000) with 21 mm outer diameter. Only these vials
guarantee optimal heat transfer between the oven block and the sample.
Use only septum seals with a PTFE insert (order. no. 6.1448.050), as these
are exposed to high temperatures. The sample vials must be tightly sealed
by using the septum closure crimpers.
Closures which are not sufficiently tight can cause significant errors in the
results. Closures which are not mounted properly may cause damage to
the injection needle.
774 Oven Sample Processor, Instructions for use
7
2 Installation
2 Installation
2.1 Setting up the instrument
Packaging
The 774 Oven Sample Processor is supplied with the accessories in separate special packages designed to ensure maximum protection. These contain shock-absorbing foam linings. As only these special packages guarantee damage-free transport of the instrument, 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 accessories list in the Instructions for Use, page 155). In case of damage see "Warranty", page 154.
Setting up
The 774 Oven Sample Processor is a rugged instrument and may be used
in rough environments such as laboratories and manufacturing 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 774 Oven Sample Processor to the power supply. Ensure that the instrument is never operated with incorrect voltage ratings and/or with fuses of an incorrect
rating, otherwise there is a fire hazard!
Setting the instrument supply voltage
Before switching on the 774 Oven Sample Processor 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:
• Disconnect line cable
Unplug the 774 Oven Sample Processor.
Remove fuse holder
Using a screw driver, loosen the fuse holder and pull it out.
774 Oven Sample Processor, Instructions for use
8
2.2 Power supply
Power switch
• 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):
2.0 A (slow) ord. no. U.600.0019
• 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 voltage. The
white arrow besides the desired voltage has to point towards the white
block mark printed on the fuse holder's panel (see below).
220 – 240 V
100 – 120 V
100
-
120 V
240 V
-
220
220 - 240 V
Power plug Fuse holder
100 - 120 V
774 Oven Sample Processor, Instructions for use
9
2 Installation
2.3 Safety considerations
• Do not operate the 774 Oven Sample Processor without protective covers.
The plug cover protects the connectors from spillage. Organic solvents
are always a potential serious fire hazard.
The protective cover of the guide head prevents the access to the stroke
path of the injection needle. Never get your hand beneath the protective
cover while operating the instrument.
• If you work with inflammable samples the 774 Oven Sample Processor
has to be operated under a safety hood. In addition to that you have to
use nitrogen or another inert gas instead of the integrated air pump. See
chapters 2.2.4 and 4.2.
• Always wear safety goggles while working with the 774 Oven Sample
Processor.
The oven can reach 250 °C and more. The heating block is covered by
a protective jacket. Keep your hands off the heated oven or the sam-
ple in work. Do not reach under the protective cover.
Caution! Just after processing sample vials may be hot, too. Even parts of
the sample rack can reach elevated temperature up to 60 °C.
• Allow the sample vials to cool off before removing vials from the rack or
detaching the sample rack .
The 774 Oven Sample Processor may be used for sample processing with
extraction methods at higher temperatures. These kinds of method require
special safety precautions.
Before working with inflammable organic solvents read the relevant
safety sheets or consult common accessible safety literature.
• Do not heat organic solvents to their flash point!
• Use nitrogen or another inert gas.
If failure or malfunctioning occurs during operation of the 774 Oven Sample
Processor, it is recommended to first search for the cause with the help of
the diagnostic functions (see Instructions for Use, page 143). If this is of no
help in rectifying the disorder or the cause of the malfunction cannot be
identified, the Metrohm Service Department should be consulted.
774 Oven Sample Processor, Instructions for use
10
2.4 Arranging the accessories
If opening the instrument is unavoidable, the following safety precautions
are to be strictly adhered to:
Before opening the instrument disconnect it from all electrical
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 acquainted 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 774 Oven Sample Processor, the sample changer and the instruments to be connected have to be
switched off, otherwise all instruments could suffer damage.
If it becomes apparent that the instrument can no longer be operated safely
it must not be used at all.
2.4 Arranging the accessories
2.4.1 Connecting the keyboard
The keyboard is connected to the
keyboard socket at the rear of the
sample changer. To disconnect
press the plug together slightly on
both sides.
774 Oven Sample Processor, Instructions for use
11
2 Installation
2.4.2 Equipping the guide head
• Screw the needle adapter (6.1808.150) onto the
bottom of the guide head.
• Attach the outlet hollow needle (6.2816.060) to the
Luer connection of the needle adapter.
• Carefully introduce the hollow injection needle
Guide head
Needle adapter
Hollow outlet
needle
Hollow injection
needle
(6.2816.050) into the guide head from above (see
arrow). Pull the needle downwards to the full extent.
• Now lead the gas inlet (6.1805.470) through the
lift head from above and screw it onto the guide
head (see arrow). Connect the other end of the
tubing to the gas outlet opening on the top of the
tower. Take care that the connections are tight.
If necessary, the injection needle may be lifted by attaching
the PTFE spacer ring (that is supplied with) to the needle.
If you wish to avoid the penetration of the sample by the
needle, you may lift the injection needle by the use of two
different M6/M8 adapters (order no. 6.1808.040 and
6.1808.090). The injection needle must only puncture the
vial's seal by a few milimeters.
2.4.3 Adjusting the sample rack
• Check the positioning of the sample rack. After switching on the 774
Oven Sample Processor place the rack on the instrument and let it move
to the first sample position by pressing the <Í> key. The circular
opening of sample position 1 of the rack must coincide with the opening
of the oven block beneath it.
• If this is not the case then loosen the three Allen screws (see diagram) on
the sample rack. Carefully adjust the upper part of the rack and then retighten the Allen screws.
• Now place a sample vial with a septum cap closure in sample position 2
and press the <Í> key again. By carefully pressing the <Ð> key to
lower the lift it is now possible to check whether the penetration needle
correctly penetrates the center of the sample vial septum and that the vial
is pressed down into the oven opening without tilting.
Warning!
Do not lower the needle too far. It must not contact the base of the vial and
become bent.
• Press the <RACK> key in order to return the sample rack and lift to the
starting position.
• Readjust the sample rack, if necessary.
774 Oven Sample Processor, Instructions for use
12
2.4 Arranging the accessories
2.4.4 Adjusting the needle position
In addition to the adjustment of the sample rack, the
Allen screws
position of the needle (radial positioning) may be
adjusted.
After the adjustment of the sample rack proceed as
follows:
1. Place a sealed beaker under the needle.
2. Lower the needle on to the seal.
3. Loosen the Allen screws of the sliding de-
4. Position the needle in the centre of the seal.
5. Fasten the sliding devices.
6. Press <RACK>. The instrument moves to
7. Remove rack.
vices.
initial position.
Positioning the needle
±1,5
111
±1
44
Distances of the guide head and rod
(in mm)
8. Check the distances according to the drawing on the right and adjust if necessary.
774 Oven Sample Processor, Instructions for use
13
2 Installation
2.4.5 Installation of the tubing system and the drying flask
A stream of gas with a constant flow rate is required to transfer the moisture
which is released when the sample is heated to a measuring vessel. You
can either use the built-in pump to supply air or use an inert gas such as nitrogen for this purpose.
Inert gas connection
Connect the inert gas to the 'Air/N
the instrument. Make sure that the pressure in the supply line is less than 1
bar. The inert gas should be dried by passing it through the drying flask.
The flow rate is measured and monitored by the 774 Oven Sample Processor. A solenoid valve is used to switch the gas flow on and off.
Air supply from the built-in pump
A stream of air can be used for the determination of chemically and thermally stable samples. The pump built into the tower of the 774 Oven Sample Processor provides a sufficiently large and stable flow rate.
It is essential that the flow of gas is dried and filtered. If the pump is used
the air is drawn in through the right-hand side of the instrument. A dust filter
(6.2724.010) should be mounted on the 'Inlet filter' connection. The gas is
dried by mounting a drying flask on the left-hand side of the instrument, as
shown in the drawing alongside.
Gas flow
The drying flask is filled with molecular sieve and the outlet tube
(6.1821.050) with its filter is fitted to the drying flask insert (6.1602.140).
2 in
Air/N
Screw the completely assembled insert onto the drying flask and attach the
two tubing connections (6.1805.520, 7 cm long) to the drying flask cap.
Place the flask in the drying flask holder and then attach the free ends of
from to
the tubing connections to the corresponding connections on the tower of
the 774 Oven Sample Processor. The tubing connected to the inlet tube in
Drying flask
the drying flask is connected to the left-hand connection marked 'from
Drying flask'. The carrier gas will stream into the head space of the flask
and penetrate the molecular sieve. Then it can stream up inside the outlet
tube and enter the tower's gas tubings via the 'from Drying flask' connector'.
The filling of the drying flask must be replaced from time to time. The interval
may vary depending on the length of use, moisture content of the gas and
atmospheric humidity. Read the information given on the label of the molecular sieve container for more details.
in' connection on the left-hand side of
2
774 Oven Sample Processor, Instructions for use
14
2.5 Integration
2.4.6 Installation of the measuring cell
Transfer hose with
outlet heating
Indicator
electrode
Septum
stopper
6.1464.320
Titration vessel
Connection for
outlet heating
r
e
t
a
e
h
t
l
e
u
t
O
Generator
electrode with
drying tube
728 Magnetic
stirrer
Stopper with
6.1446.170 O-ring
Example: 6.1464.320 Coulometer titration vessel
Install the necessary accessories as shown in
the diagram alongside.
The fastening screws can be used to permanently fix the whole assembly in position.
If you wish to automate the reagent changing
process (aspiration and dosing) then the Coulometer titration vessel with two side-mounted
threaded openings (6.1465.320) should be
used.
If volumetric KF determinations are to be carried out a suitable titration vessel should be
selected (see Metrohm accessories catalog)
together with the KF titration vessel upper part
(6.1414.030). Instead of the 6.1446.170 stopper use the nipple and O-ring of the
6.2730.030 stopper to introduce the transfer
hose into the titration vessel.
Fastening screws
2.5 Integration
Cables
Connecting peripheral instruments to the 774 Oven Sample Processor requires Metrohm cables. Otherwise 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. Look at the cable ends. For example:
All instruments have to be switched off before they are connected.
Otherwise the instruments could be damaged.
Titrino B
692 / 712 / 713
774 Oven Sample Processor, Instructions for use
15
2 Installation
The 774 Automation System
700 Dosino 685 Dosimat
756 Coulometer
684
737
701
...
784
PC software
Metrohm-
instruments
729
729 Dosimat Interface
External Bus
Coulometer
Titrino
family
other
instruments
printers
Seiko
Citizen
Epson
HP
IBM
…
RS 232
774
774 Oven Sample Processor
2.5.1 Remote connections
774 Oven Sample Processor — 756 Coulometer
for coulometric determinations
Remote
726 Titroprocessor
other
instruments
6.2125.110
cable (RS232)
774
756
6.2141.020
cable (remote)
Control of the 756 Coulometer is carried out via the control lines of the remote connection.
While a sequence is being processed the 774 Oven Sample Processor can,
via the serial RS232 interface, cause the 756 Coulometer to load a particular method. When drawing up a report the 756 Coulometer automatically
obtains the temperature of the 774 Oven Sample Processor via the RS232
connection.
774 Oven Sample Processor, Instructions for use
16
2.5 Integration
Control commands of the 774:
CTL:Rm : START Gerät1 starts Coulometer
CTL:Rm : *************1 "
CTL:RS &U.R.N loads a method in the Coulometer
CTL:RS "774BLANK"..$G here e.g. "774BLANK"
Scanning the remote lines of the 774:
SCN:Rm : **0**010 waits for 'cond. ready'
SCN:Rm : *****000 waits for end of determination
774 Oven Sample Processor — 737 Coulometer
for coulometric determinations
774
737
6.2141.000 cable (remote)
The 737 Coulometer is completely controlled via the remote lines.
Control commands:
CTL:Rm: *********1**** starts Coulometer with
CTL:Rm: *********0**** a start impulse
Scanning via remote lines:
SCN:Rm : 10000100 waits for 'cond. ready'
774 Oven Sample Processor — 7xx Titrino
for volumetric KF titrations
774
774 Oven Sample Processor, Instructions for use
6.2141.020
cable (remote)
758
17
2 Installation
Control commands:
CTL:Rm : START Gerät1 starts Titrino
CTL:Rm : ***********1** advance impulse / ENTER
Scanning via remote lines:
SCN:Rm : ****1000 waits for end of titration (EOD-impulse)
SCN:Rm : *****010 waits for 'cond. ok'
In principle it is possible to use an additional RS232 connection to automatically load a particular method in the Titrino while a sequence is being
processed. Please refer to the example of the remote connection given for
the 756 Coulometer on the previous page.
774 Oven Sample Processor — 796 Titroprocessor
for volumetric KF titrations
6.2125.110
cable (RS232)
6.2141.020
cable (remote)
or
If connected to a 774 Oven Sample Processor the 796 Titroprocessor takes
over the functions of the control instrument itself (Master). The communication between the 774 Oven Sample Processor and the 796 Titroprocessor
can be solved in any manner.
If a remote connection is used (6.2141.020 cable) the input and output lines
0…7 can be used as required. However, it is then not possible to start a
774 Oven Sample Processor method. See page 79ff for the communication
commands.
A serial RS232 connection between the 796 Titroprocessor and the 774
Oven Sample Processor has the advantage that the Titroprocessor as control unit can access all internal functions except starting or loading a
method in the 774 Oven Sample Processor. Please refer to the description
of the Metrohm remote language and the 774 remote control tree on page
98ff.
774 Oven Sample Processor, Instructions for use
18
2.5 Integration
2.5.2 External bus connections
If a KF Titrino or a Coulometer which does not support automatic solvent
changing is connected to the 774 Oven Sample Processor then this can be
carried out with the help of a 700 Dosino. 685 Dosimats can also be used
for the addition of solvents. 700 Dosinos or 685 Dosimats are connected to
the 774 Oven Sample Processor via the so-called 'External Bus'.
A 729 Dosimat interface can be used to connect up to 4 dosing devices to
the 'External Bus' interface. Up to 3 Dosimat interfaces can be switched in
line (cascaded) and equipped with further dosing instruments. The instrument address must always be set correctly at the interfaces. In this way it is
possible to operate up to 12 dosing instruments directly with the 774 Oven
Sample Processor with the aid of the DOS command.
Dos. 1
685
Dos. 2
6.2134.000 cable
774
6.2135.000 cable
729
Dos. 4
Dos. 3
EBus
address 1
Addresses:
'External Bus'-
address
774 Oven Sample Processor 0
1st interface 1 Dos. 1 … Dos. 4
2nd interface 2 Dos. 5 … Dos. 8
3rd interface 3 Dos. 9 … Dos. 12
700
Dosing instrument
774 Oven Sample Processor, Instructions for use
19
2 Installation
2.5.3 Serial connection (RS232)
Many different instruments may be connected via the serial RS232 interface. In addition to all Metrohm instruments that support the Metrohm remote control language (see page 101ff) any printer with serial interface (or
parallel interface and parallel/serial converter) or a personal computer (PC)
may be connected. Any other measuring instrument may be controlled via
RS232 interface, as long as it supports serial data transmission.
6.2125.060 cable
Printer cables see page. 20f
In order to guarantee safe data transmission, it is important to set the same
RS232 interface parameters correctly for both instruments connected (see
page 21f).
Control commands (examples):
CTL:RS &M;$G starts a Metrohm instrument
CTL:RS &M;$S stops a Metrohm instrument
PRINT: config
Scanning input data (example):
SCN:RS : *R" waiting for readiness of a Metrohm instru-
Information about the settings and cables required for connecting a printer
is given in the following section.
prints a configuration report to a printer or
PC
ment
774 Oven Sample Processor, Instructions for use
20
2.5 Integration
2.5.4 Connecting a printer
Printers with the following printer emulations may be connected:
IBM IBM Proprinter and printers with IBM emulation
Epson Epson printers and printers with Epson emulation
Seiko Seiko printer DPU-411/414
Citizen Citizen printer IDP560 RS
HP
HP printers and compatibles with HP PCL3 emulation
If you connect a printer not listed in the following table, be sure that it is able
to emulate Epson or IBM Proprinter mode.
Use the 6.2125.050 cable for connecting a printer with built-in serial interface. Printers with parallel interface require the 2.145.0300 serial/parallel
converter and 6.2125.020 cable.
Before connecting a printer to the RS232 interface, switch off the
774 Oven Sample Changer.
The parameters of the RS232 interface are accessible in the configuration
menu under '>RS232 settings'.
The following table lists the information necessary for connecting a printer:
Printer type Cable RS232 Settings Settings on Printer
IBM Proprinter 6.2125.050
Seiko
6.2125.020
DPU-411
Seiko
6.2125.130
DPU-414
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: IBM
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: Seiko
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: Seiko
see printer manual
DIP switch settings:
DIP01 DIP02
on
off
12345678
The 7-bit ASCII character is set automatically to the specific national character set
according to the selected dialog language.
Recommended DIP switch settings
Dip SW-1 Dip SW-2 Dip SW-3
1 OFF ON ON
2 ON OFF ON
3 ON ON ON
4 OFF ON ON
5 ON ON OFF
6 OFF ON ON
7 ON OFF ON
8 ON OFF ON
The 7-bit ASCII character is set automatically to the specific national character set
according to the selected dialog language.
123456
774 Oven Sample Processor, Instructions for use
21
2 Installation
Printer type Cable RS232 Settings Settings on Printer
Citizen
IDP560-RS
6.2125.050
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set:Citizen
DIP switch settings:
on
off
12345678
The 7-bit ASCII character is altered to the
specific national character set by setting
the jumpers J1 and J2 as follows:
J1 J2 character set
open open USA
closed closed Great Britain
closed. open France
open closed Germany
No Spanish character set available
(French may be best).
Epson
6.2125.040
with 6-pole
round plug
Epson
6.2125.050
with additional
serial interface
#8148
Epson LX-300 6.2125.050
HP Deskjet
with built-in
serial interface
6.2125.050
or cable 25pole neg. /
9-pole pos.
(e.g. HP
C2933A)
HP Laserjet
with built-in
serial interface
cable 25pole neg. /
9-pole pos.
(e.g. HP
C2933A)
HP Deskjet /
Laserjet
with parallel
interface
6.2125.020
+ serial/
parallelconverter
2.145.0300
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: Epson
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: Epson
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: Epson
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: HP
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: HP
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
character set: HP
DIP switch settings:
SW1 SW2
on
off
12345678
12345678
DIP switch settings on the Interface:
SW1 SW2
on
off
123456
12345678
see printer manual
DIP switch settings :
A B
on
off
12345678
12345678
see printer manual
see printer manual*
* character set PC-8 is required.
PCL3 command: esc(10U
774 Oven Sample Processor, Instructions for use
22
3.1 Configuration
3 Introduction
3.1 Configuration
The 774 Oven Sample Processor must be configured correctly before it is
used for the first time. This includes both the basic settings with the oven
settings and the configuration of the sample rack and the peripheral devices which are connected. All these settings are accessible via the configuration menu which can be opened with the <CONFIG> key. It is arranged in various submenus according to subject. Navigating (selecting the
individual settings) in the menu is carried out with the cursor keys (<Ð>,
<Ï>) and is also possible with the <HOME>, <END> and <ENTER>
keys. Submenus and main menus are exited with the <QUIT> key. In
many menu entries the <SELECT> key can be used to select the required
entry from a list of entries. These menu items are marked with a colon (:).
Further details are given on page 58.
When the configuration has been altered a RESET should be carried out
with <CLEAR> or the oven sample changer should be switched off and
on in order to ensure that the alterations become effective.
3.1.1 Basic settings
The basic settings which can be set in the submenu '>auxiliaries' include:
• dialog language
• display contrast
• beeper on/off for warnings
• Instrument identifier (instrument name or identification)
• program version
• maximum lift height and way
• beaker sensor on/off.
dialog
The dialog language can be selected from 'deutsch, english, français,
español'.
display contrast
The display contrast can be set on a scale from 0 (low contrast) to 7 (high
contrast).
beeper on/off
With error messages or when a value has been entered and not confirmed
with <ENTER> (and as a result is not accepted) then an acoustic signal is
produced. This signal can be switched off.
774 Oven Sample Processor, Instructions for use
23
3 Introduction
device label
In order to be able to identify each particular laboratory instrument unambiguously (required by GLP) the sample changer can be given an 8-character
identifier made up of letters and/or numbers. Text input is described on
page 59.
program version
The program version (instrument software) cannot be altered. It is shown in
the configuration menu for information.
max. lift way
The maximum lift way is an important safety entry. If a correct entry is made
this ensures that the lift with the working head cannot be moved down too
far; this could cause damage to the needle or the sample vessel. The lowest lift position to be reached can be entered in mm (measured from the
upper stop position).
A convenient way of determining this position is to set the required height
manually (normal state) with the <Ð> and <Ï> keys. The configuration
menu is then opened and the current lift position in the display can be accepted in the menu entry 'max. lift way' with the <CLEAR> key.
Important: the entered value only becomes effective after a RESET or
when the instrument is switched off and then on again.
beaker sensor
The tower of the 774 Oven Sample Processor is equipped with an infraredbeaker sensor which detects the presence of a sample vial in front of the
tower. If the beaker sensor is switched on then this test will be carried out
after each MOVE command.
This entry also only becomes effective after a RESET or when the instrument is switched off and then on again.
3.1.2 Oven settings
The basic settings for the oven affect the various temperatures.
initial temperature
Entry of an initial temperature means that the oven is heated up to the set
temperature immediately after the 774 Oven Sample Processor is switched
on. The initial temperature can also be used as a parameter for the
HEATER command. (HEATER:init°C)
max. temperature
The maximum temperature is used as a safety setting. The entered value
cannot be exceeded. If the oven reaches the maximum temperature during
heating up then an error message is produced and the oven heating is
switched off. This emergency stop prevents the sample from being overheated.
temp. correction
The temperature correction allows the temperature control to be adjusted.
This can compensate for any temperature difference which may occur between the oven temperature and the sample temperature. The temperature
correction has a direct effect on the temperature control. The temperature
which is displayed is always the corrected oven temperature.
24
774 Oven Sample Processor, Instructions for use
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