Metrohm 813 User manual

CH-9101 Herisau/Switzerland
Phone [phone]
Fax [phone]
E-Mail [email protected]
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813 Compact Autosampler
Program version 5.813.0010
Instructions for use
8.813.1003 06.2001 / dm

D. Möckli
Teachware
Metrohm Ltd.
Oberdorfstr. 68
CH-9100 Herisau
1st Edition 2001
Copyright © 2001 by Metrohm Ltd. All rights reserved.
This manual was carefully produced. Nevertheless the author does not warrant the
information contained herein to be free of errors. The author appreciates your
comments and feedback.
© Metrohm Ltd. 2001
Printed in Switzerland

Table of content
1Introduction ......................................................1
1.1 Instrument description .................................................................................1
1.2 Parts and controls.........................................................................................2
1.3 Rear view........................................................................................................4
1.4 The keyboard .................................................................................................5
2Installation........................................................6
2.1 Setting up the instrument.............................................................................6
2.1.1 Packaging ..................................................................................................6
2.1.2 Delivery check ............................................................................................6
2.1.3 Location......................................................................................................6
2.2 Mains connection ..........................................................................................7
2.2.1 Setting the mains voltage...........................................................................7
2.2.2 Fuses..........................................................................................................8
2.2.3 Mains cable and mains connection...........................................................8
2.2.4 Switching the instrument on/off..................................................................9
2.3 Attaching the accessories............................................................................9
2.3.1 Connecting the keyboard...........................................................................9
2.3.2 Installing the plug cover .............................................................................9
2.3.3 Installing the needle .................................................................................10
2.3.4 Installing the splash protection ................................................................11
2.3.5 Placing the sample rack...........................................................................12
2.3.6 Adjusting the sample rack .......................................................................12
2.3.7 Tubing connections..................................................................................14
2.3.8 Tubing connection to Metrohm 761 / 790 IC–Systems ...........................15
2.3.9 Tubing connection to a Metrohm 747 VA Stand......................................16
2.3.10 Tubing connection to a Metrohm Computrace 757.................................16
2.4 Instrument connections..............................................................................17
2.4.1 Remote interface ......................................................................................17
2.4.2 Interconnection with Metrohm IC systems...............................................17
2.4.3 Interconnection with a Metrohm 746 VA Trace Analyzer .........................18
2.4.4 Interconnection with a Metrohm 757 VA Computrace .............................19
2.4.5 Interconnection with other instruments ....................................................19

3Operation ........................................................20
3.1 Keyboard functions.................................................................................... 20
3.2 Configuration .............................................................................................. 21
3.2.1 Course of configuration ...........................................................................23
3.3 RAM initialization........................................................................................ 24
3.4 The methods ............................................................................................... 25
3.5 The Metrohm IC control software ............................................................. 27
3.5.1 Operational conditions.............................................................................27
3.6 Modular Metrohm IC System 732/733 ....................................................... 28
3.7 Metrohm 746 VA Trace Analyzer ............................................................... 28
3.7.1 Monitoring ................................................................................................28
3.7.2 Command sequence ...............................................................................28
3.7.3 Conditions to be met ...............................................................................29
4Appendix..........................................................30
4.1 Error Messages........................................................................................... 30
4.2 Sequences................................................................................................... 31
4.3 Technical specifications ............................................................................ 35
4.4 Maintenance and servicing........................................................................ 37
4.4.1 Maintenance by Metrohm service ...........................................................37
4.4.2 Care of the unit.........................................................................................37
4.4.3 Replacing the pump tubing .....................................................................37
4.5 Warranty and conformity ........................................................................... 39
4.5.1 Warranty ...................................................................................................39
4.5.2 Certificate of Conformity and System Validation .....................................40
4.6 Standard equipment ................................................................................... 42
4.7 Optional accessories.................................................................................. 46
5Index................................................................48

Table of Figures
Fig. 1 Side view ........................................................................................................ 2
Fig. 2 Rear view........................................................................................................ 4
Fig. 3 Keyboard........................................................................................................ 5
Fig. 4 Setting the mains voltage .............................................................................. 8
Fig. 5 Keyboard connection..................................................................................... 9
Fig. 7 Installing the splash protection.................................................................... 11
Fig. 8 Sample rack placing .................................................................................... 12
Fig. 9 Installing the pump tubing ........................................................................... 15
Fig. 10 Connection of a 747 VA Stand..................................................................... 16
Fig. 11 Measuring head of the747 VA Stand ........................................................... 16
Fig. 12 Interconnection with 761 or 790 IC System ................................................ 17
Fig. 13 Interconnection with a modular Metrohm IC System .................................. 18
Fig. 14 Interconnection with a Metrohm 746 VA Trace Analyzer ............................. 18
Fig. 15 Interconnection with 757 VA Computrace................................................... 19
Fig. 16 Configuration................................................................................................ 23
Fig. 17 Time program of the IC control software..................................................... 27

1 Introduction
813 Compact Autosampler 1
1 Introduction
1.1 Instrument description
The 813 Compact Autosampler can be used for automat-
ing different tasks, e.g. ion chromatographic determinations with
the Metrohm IC system instruments or voltammetric determina-
tions with the Metrohm 746 Trace Analyzer or 757 VA Com-
putrace . The sample rack provided may hold up to 36 vials of 2.5
or 11 mL volume respectively. Sample tubes made of polypropyl-
ene are standard. To protect the samples from external contami-
nation, the tubes can be hermetically sealed.
Sample introduction from the 813 Compact Autosampler is
achieved by means of its integrated peristaltic pump. The sample
is conveyed by the pump through the capillary into e. g. the sam-
ple loop of the injector located within an ion chromatograph. A
PEEK needle for sealed or a PEEK tube for open sample tubes
can be used alternatively.
Preprogrammed methods for the most common modes of opera-
tion allow to use the 813 Compact Autosampler directly, without
programming effort.

1.2 Parts and controls
2 813 Compact Autosampler
1.2 Parts and controls
DE S F USI B LES DE 250 V
USEONLYWITH 250V
UNIQUEMENT AVEC
FUSES/EMPLOYER
100-120V
220-240V
1
Metrohm
2
3
4
56 7
8
9
1
0
11
1
3
1
4
1
5
1
7
1
8
1
9
21
22
23
24
25
2
0
1
2
1
6
26
Fig. 1 Side view
Safety note:
Never operate the instrument without splash protection and plug
cover being mounted.
The plug cover prevents any contamination of the connectors,
caused by spilled solvents or chemicals.

1 Introduction
813 Compact Autosampler 3
1
Splash protection 6.2751.040
Must be installed always in operation!
14
Holding clamp
For locking the tubing cartridge into
place
2
Needle
PEEK needle 6.1835.020 or PEEK
tube 6.1835.010 or 6.1835.030
15
Snap-action lever
For releasing the tubing cartridge
3
Lift
16
Screw thread for splash
protection
4
Steel holder 4.766.4330
attached (part of 6.2833.000 Needle
holder)
17
PEEK capillary 6.1831.060 or
6.1822.410 (1 m or 1.2 m)
For conveying the sample to e.g. an
injection valve
5
PEEK compression fitting
4.766.4320
for connection of PEEK capillary
7
(part of 6.2833.000 Needle holder)
18
Tower
6
PEEK compression fitting
6.2744.010
19
Remote connection
7
PEEK capillary 6.1831.050
(40 cm)
connection needle – pump tubing
20
Plug cover 6.2752.010
8
Pump tubing 6.1826.040
For conveying the sample
21
Fuse holder
Changing the fuses, see section 2.2.2
9
Screw thread for splash
protection
22
Mains connection plug
Mains connection, see section 2.2.3
10
Mounting pin
For attaching the tubing
cartridge
23
Mains switch
For switching the instrument on/off:
I= ON 0= OFF
11
Tubing cartridge 6.2755.000
For 6.1826.0X0 pump tubing
6.1826.0X0
24
Sample rack 6.2041.7500
12
Pump drive
Roller head with contact rollers
25
PP sample tube 6.2743.050
(can be sealed with 6.2743.060 PE
caps)
13
Contact pressure lever
For adjusting the contact pressure
26
Needle guide

1.3 Rear view
4 813 Compact Autosampler
1.3 Rear view
9
27
28
Made by Metroh m Herisau Switze rland
Keyboard
Type 1.813.
9
11
16 16
18
25
20
24
Fig. 2 Rear view
9
Mounting screws for
splash protection
24
Sample rack 6.2041.750
11
Tubing cartridge
6.2755.000
For 6.1826.0X0 pump tubing
25
PP sample tubes 6.2743.050
(can be sealed with 6.2743.060 PE
caps)
16
Mounting screws for
splash protection
27
Serial number
18
Tower
28
Keyboard connection
20
Plug cover 6.2752.010

1 Introduction
813 Compact Autosampler 5
1.4 The keyboard
813 Compact Autosampler
START
HOLD
RESET
STOP
Metroh m
6.2142.110
Fig. 3 Keyboard
• The <START> key starts a sample series or
continues an interrupted series.
• The <STOP> key terminates a sample series
or resets (if pressed twice) the 813 Compact
Autosampler (RESET).
• The <HOLD> key interrupts the course of a
sample series and establishes the 'HOLD'
state. The green LED blinks. With the
<START> key the interrupted sample series
can be continued.
• The green LED indicates the status of the
Autosampler.
- The LED is lit in the 'ready' state.
- It blinks steady during the course of a
method.
- It blinks in fast frequency when a series is
interrupted ('HOLD' state).
• The red LED indicates error states or parame-
ter settings.
- If an error occured the type of error is indi-
cated by the number of blinks, see Ap-
pendix, Error messages.

2.1 Setting up the instrument
6 813 Compact Autosampler
2 Installation
2.1 Setting up the instrument
2.1.1 Packaging
The 813 Compact Autosampler is supplied together with the
separately packed accessories in special packagings containing
shock-absorbing foam linings designed to provide excellent pro-
tection. The actual instrument is packed in an evacuated polyeth-
ylene bag to prevent the ingress of dust. Please store all these
special packagings as only they can assure damage-free trans-
port of the instrument.
2.1.2 Delivery check
After receipt, immediately check whether the shipment is com-
plete and undamaged (compare with delivery note and list of ac-
cessories in section 4.6). In the case of transport damage, see in-
structions in section 4.5.1 "Warranty".
2.1.3 Location
Position the instrument in the laboratory at a location convenient
for operation, free from vibrations and protected against a corro-
sive atmosphere and contamination by chemicals.
Do not operate the 813 Compact Autosampler without splash
protection
1
and plug cover
20
being installed!
Take precautions to ensure that any leaks from pump tubings or
connections cannot cause more damage.
Take precautions to ensure that any leaks from pump tubings or
connections cannot cause more damage.

2 Installation
813 Compact Autosampler 7
2.2 Mains connection
Follow the instructions below for connecting to the power
supply. If the instrument is operated with the mains voltage set
wrongly and/or wrong mains fuse there is a danger of fire!
2.2.1 Setting the mains voltage
Before switching on the 813 Compact Autosampler for the first
time, check that the mains voltage set on the instrument (see Fig.
4) matches the local mains voltage. If not, reset the mains voltage
on the instrument as follows:
1 Disconnect mains cable
Disconnect mains cable from mains connection plug
22
of the
813 Compact Autosampler.
2 Remove fuse holder
Using a screwdriver, loosen fuse holder
21
beside the mains
connection
22
and take out completely.
3 Check fuse
Carefully take the fuse installed for the desired mains voltage out
of fuse holder
21
and check its specifications (the position of the
fuse in the fuse holder is marked by the white arrow imprinted
next to the mains voltage range):
100…120 V 0.5 A (slow-blow)
Metrohm-Nr. U.600.0013
220…240 V 0.25 A (slow-blow)
Metrohm-Nr. U.600.0010
4 Insert fuse
Change fuse if necessary and reinsert in fuse holder
21
.
5 Install fuse holder
Depending on the desired mains voltage, insert fuse holder
21
in the 813 Compact Autosampler so that the corresponding
mains voltage range can be read normally and the adjacent
white arrow points to the white bar imprinted on the right side of
the fuse holder (see Fig. 4).

2.2 Mains connection
8 813 Compact Autosampler
23
22
21
220 -240 V
100 -120 V 220 -240 V
100 -120 V
Fig. 4 Setting the mains voltage
2.2.2 Fuses
One of the two fuses 0.5 A/slow-blow for 100…120 V or 0.25
A/slow-blow for 220…240 V is installed in fuse holder
21
of the
813 Compact Autosampler as standard
Ensure that the instrument is never put into operation with fuses
of another type, otherwise there is danger of fire!
For checking or changing fuses, proceed as described in section
2.2.2.
2.2.3 Mains cable and mains connection
Mains cable
The instrument is supplied with one of three mains cables
• 6.2122.020 with plug SEV 12 (Switzerland, …)
• 6.2122.040 with plug CEE(7), VII (Germany, …)
• 6.2133.070 with plug NEMA 5-15 (USA, …)
which are three-cored and fitted with a plug with an earthing pin.
If a different plug has to be fitted, the yellow/green lead (IEC
standard) must be connected to protective earth (protection class
1).
Any break in the earthing inside or outside the instrument can
make it a hazard!
Mains connection
Plug the mains cable into mains connection plug
22
of the 813
Compact Autosampler (see Fig. 4).
220 – 240 V
100 – 120 V
21 Fuse holder
22
Mains connec-
tion plug
23
Mains switch

2 Installation
813 Compact Autosampler 9
2.2.4 Switching the instrument on/off
The 813 Compact Autosampler is switched on and off using the
mains switch
23
.
2.3 Attaching the accessories
For attaching the accessories at the 813 Compact Autosampler,
proceed in the order described below.
2.3.1 Connecting the keyboard
1
2
Connecting the keyboard
Connect the 6.2142.110 keyboard
to the keyboard connection
28
"Keyboard". For disconnection,
press the plug together slightly on
both sides.
Switch on the instrument
Switch on the 813 Compact
Autosampler with mains switch
23
.
The instrument is initialized and
the lift is raised completely. The
green LED lights up.
MadebyMetrohmHeri s au Switzerland
Keyboard
Type 1. 76 0. 001 0 Nr. 00 10 /01104
Fig. 5 Keyboard connection
2.3.2 Installing the plug cover
To prevent any contamination of the mains and remote connec-
tion by spilled solvents or chemicals, the 6.2752.010 plug cover
must always be installed when operating the 813 Compact
Autosampler!
Install the plug cover
20
in the corresponding guide groove
above mains connection plug
22
and remote connection
19
(see
Fig. 1 and Fig. 2).

2.3 Attaching the accessories
10 813 Compact Autosampler
2.3.3 Installing the needle
1 Remove PEEK compression fitting 5
Remove PEEK compression fitting
5
screwed onto the needle
holder
4
.
2 Insert needle
• Needle
2
(6.1835.010 PEEK needle or 6.1835.020 or
6.1835.010 PEEK tube) is inserted a short distance into the
opening of steel holder
4
.
• Push PEEK round seal
29
over needle
2
from above. The
smaller end of the seal must face upwards.
3 Fix needle
• Screw PEEK compression fitting
5
into steel holder
4
while
pressing needle
2
gently upwards from below.
• Tighten compression fitting
5
in steel holder
4
by hand
(never use tools!).
If you are using the 6.1835.020 or 6.1835.030 PEEK tube as needle, the
sample tubes must not be sealed with caps because they cannot be
pierced by the PEEK tube and this could damage the tube!
2 PEEK needle (6.1835.010) or PEEK
tube (6.1835.020 or 6.1835.030)
4 Steel holder (4.766.4330)
(part of 6.2833.000 Needle holder)
5 PEEK compression fitting
(4.766.4320)
(part of 6.2833.000 Needle holder)
6 PEEK compression fitting
(6.2744.010)
7 PEEK capillary (6.1831.050)
29 PEEK ferrule
2
4
5
6
7
2
5
29
Fig. 6 Needle installation

2 Installation
813 Compact Autosampler 11
2.3.4 Installing the splash protection
To avoid any danger of injury by the needle, the 6.2751.070 splash
protection must always be installed when operating the 813 Compact
Autosampler!
1 Remove holding screws
Remove the holding screws
16
and the washer mounted on the
screw threads
9
at tower
18
using the 6.2621.100 Allen key.
2 Remove protective film from splash protection
Remove the plastic film glued on both sides of the splash
protection
1
.
3 Install splash protection
Attach splash protection
1
onto the screw threads
9
and
16
at
the tower
18
and fix it with the holding screws
9
and the washer
using the 6.2621.100 Allen key.
9
16
1
Fig. 7 Installing the splash protection
1Splash protection
6.2751.040
9Holding screw
16 Holding screw

2.3 Attaching the accessories
12 813 Compact Autosampler
2.3.5 Placing the sample rack
1
2
Place sample rack
Place sample rack
24
on the
turntable of the 813 Compact
Autosampler acc. to Fig. 8.
Initialize rack
Press <RESET> to move the
rack to the home position, in
which the magnetic code can
be read (coding magnet 30).
30
Fig. 8 Sample rack placing
2.3.6 Adjusting the sample rack
If a new sample rack is placed on the 813 Compact Autosampler
for the first time, it must be adjusted. Make sure you have
mounted a steel needle or a PEEK needle before. Proceed as fol-
lows:
1 Place sample rack
Place empty sample rack
24
on the turntable of the 813 Com-
pact Autosampler and switch off the instrument.
2 Switch on the instrument
Keep the <HOLD> key pressed and simultaneously press the
mains switchon the right hand sideof the 813 Compact Auto-
sampler. The instrument is initialized and the needle is placed
above rack position 1. Press the <START> key. The green LED
is now blinking twice.

2 Installation
813 Compact Autosampler 13
3 Check needle position
• Press <HOLD> until the needle
2
is about 1 cm above the
upper level of the sample rack
24
.
• Check needle position: If the needle 2cannot be lowered
unhindered through the upper hole of the rack position 1,
continue directly with point 4.
• Press <HOLD> once and continue lowering the needle by
pressing <HOLD> again until the needle
2
stops.
• Check needle position: If the needle
2
points to the middle of
lower hole of the rack position 1, the sample rack must not be
adjusted (continue directly with point 5).
4 Adjusting the sample rack
• Loosen the four adjusting screws
33
on the lower level of the
sample rack using the 6.2621.100 Allen key .
• Carefully turn the two upper levels of the sample rack
27
by
hand until the lowered needle
2
is exactly in the middle of the
lower hole at the rack position 1.
• Tighten the adjusting screws
33
.
5 Move to rest position
Press <STOP> twice to move the sample rack to the initial
position.

2.3 Attaching the accessories
14 813 Compact Autosampler
2.3.7 Tubing connections
Pump tubings are consumable material with a lifetime which
depends on the contact pressure (see section 4.4 Maintenance
and servicing). This is why the tubing cartridges should be
raised completely by loosening snap-action lever 15 on the
right-hand side if the pump is to remain switched off for a
considerable length of time (the set contact pressure remains
unchanged).
The 6.1826.0X0 pump tubing is made of PVC and must not be
used for rinsing with solutions which contain acetone. In such
cases, rinse with different pump tubing or a different pump.
For transferring the sample from the 813 Compact Autosampler
to an injection valve the following tubing connections must be
made:
1 Install pump tubing
• Release tubing cartridge
11
from holding clamp
14
by
pressing down snap-action lever
15
and remove it from
mounting pin
10
on the 813 Compact Autosampler (see Fig.
9).
• Press contact pressure lever
13
on the tubing cartridge down
as far as it will go.
• Insert pump tubing
8
in the tubing cartridge
11
as shown in
Fig. 9. The black stopper
32
must click into the correspond-
ing holder on the left-hand side of the tubing cartridge.
• Place the tubing cartridge
11
on mounting pin
10
and press
down on the right-hand side until snap-action lever
15
clicks
into position on holding clamp
14
. Take care that no kinks are
formed in the pump tubing.
2 Connection needle – pump tubing
• Mount a PEEK compression fitting
6
on both ends of the
PEEK capillary
7
.
• Screw the PEEK capillary
7
with the PEEK compression fitting
6
on to the PEEK compression fitting
5
already mounted on
needle holder
4
(see Fig. 9).
• Screw a coupling
31
on to the PEEK compression fitting at
the other end of PEEK capillary
7
.
• Push coupling
31
on to the inlet end of the pump tubing
8
(see Fig. 9).