Metrohm 861 User Manual
861 Advanced Compact IC
CH-9101 Herisau/Switzerland
E-Mail info@metrohm.com
Internet www.metrohm.com
Instructions for Use
8.861.1033
CH-9101 Herisau/Switzerland
E-Mail info@metrohm.com
Internet www.metrohm.com
861 Advanced Compact IC
8.861.1033 Instructions for Use
8.861.1033 05.2005 / chs
Teachware
Metrohm AG
Oberdorfstrasse 68
CH-9101 Herisau
teachware@metrohm.com
1. Edition 2005
These instructions are protected by copyright. All rights reserved.
Although all the information given in these instructions has been checked with great care, errors
cannot be entirely excluded. Should you notice any mistakes please inform the author at the
address given above.
Table of contents
Table of contents
1 Introduction ................................................................ 1
1.1 Instrument description ................................................................................1
1.2 Parts and controls .......................................................................................3
1.2.1 Front.................................................................................................................... 3
1.2.2 Rear panel .......................................................................................................... 4
1.2.3 Interior 2.861.0010.............................................................................................. 5
1.2.4 Interior 2.861.0020.............................................................................................. 7
1.2.5 Interior 2.861.0040.............................................................................................. 9
1.3 Information on the Instructions for Use...................................................11
1.3.1 Organization .....................................................................................................11
1.3.2 Notation and pictograms.................................................................................. 12
1.4 Safety notes ...............................................................................................13
1.4.1 Electrical safety................................................................................................. 13
1.4.2 General precautionary rules ............................................................................. 13
2 Installation ............................................................... 14
2.1 Overview ....................................................................................................14
2.1.1 Flow chart ......................................................................................................... 14
2.1.2 Connections in the 861 Advanced Compact IC .............................................. 14
2.2 Setting up the instrument..........................................................................16
2.2.1 Packaging.........................................................................................................16
2.2.2 Check................................................................................................................ 16
2.2.3 Location ............................................................................................................ 16
2.3 Attaching the accessories.........................................................................17
2.3.1 Connection of detector block........................................................................... 17
2.3.2 Connection of syringe and aspirating tubing...................................................18
2.3.3 Connection of the drain tube for the inner compartment ................................ 18
2.3.4 Connection of the drain tube for bottle rack ....................................................18
2.3.5 Connection of PEEK capillaries........................................................................ 18
2.3.6 Filter unit PEEK ................................................................................................. 19
2.4 Mains connection ......................................................................................21
2.4.1 Setting the mains voltage................................................................................. 21
2.4.2 Fuses ................................................................................................................ 22
2.4.3 Mains cable and mains connection ................................................................. 22
2.4.4 On/off switching of the instrument ...................................................................22
2.5 Connection to PC ......................................................................................23
2.5.1 Connecting cable .............................................................................................23
2.5.2 Software installation.......................................................................................... 23
2.5.3 First Login ......................................................................................................... 24
2.5.4 Create a system ............................................................................................... 24
2.6 High-pressure pump .................................................................................25
2.6.1 Removing the transport security screws.......................................................... 25
2.6.2 Installing the pulsation dampener.................................................................... 25
2.6.3 Connecting the eluent bottle ............................................................................ 26
2.6.4 Deaerating the pump and rinsing the pulsation dampener............................. 28
2.7 Precolumns and separating columns ......................................................30
2.7.1 Precolumns....................................................................................................... 30
2.7.2 General information on separating columns ................................................... 31
2.7.3 Selecting the sample loop................................................................................ 31
2.7.4 Installation of the separating column without suppressor module «MSM II» .. 32
2.7.5 Installation of the separating column with suppressor module «MSM II» ....... 33
861 Advanced Compact IC / Instructions for Use 8.861.1033
I
Table of contents
2.8 Suppressor module «MSM II» ...................................................................34
2.8.1 General information on suppressor module «MSM II» .................................... 34
2.8.2 Preparation of the peristaltic pump.................................................................. 35
2.8.3 Connection of supply bottles ........................................................................... 38
2.8.4 Connection of the suppressor module «MSM II»............................................. 40
2.9 853 CO2 Suppressor..................................................................................42
2.9.1 853 CO2 Suppressor - Installation ................................................................... 42
2.9.2 853 CO2 Suppressor – Mains connection ....................................................... 42
2.9.3 853 CO2 Suppressor – Connection to 861 ...................................................... 42
2.9.4 853 CO2 Suppressor – Tubing connection...................................................... 43
2.10 Putting into operation................................................................................43
2.10.1 Putting into operation without suppressor module «MSM II» .......................... 43
2.10.2 Putting into operation with suppressor module «MSM II» ............................... 45
2.11 Connection of external devices ................................................................48
2.11.1 Connection of the 838 Advanced Sample Processor ..................................... 48
2.11.2 Connection of the 813 Compact Autosampler ................................................ 50
3 Operation .................................................................. 53
3.1 «IC Net» - Terms.........................................................................................53
3.2 Measuring operation .................................................................................53
3.2.1 Opening a system ............................................................................................ 53
3.2.2 Connect a system ............................................................................................ 54
3.2.3 Instrument icon................................................................................................. 54
3.2.4 Hardware start/stop and baseline recording ................................................... 55
3.2.5 Determination start/stop................................................................................... 55
3.3 Settings ......................................................................................................56
3.3.1 Instrument control for connected system ........................................................ 56
3.3.2 Hardware settings ............................................................................................ 62
4 Notes - Maintenance - Faults ................................... 66
4.1 Practical notes on ion chromatography ...................................................66
4.1.1 Separating columns ......................................................................................... 66
4.1.2 High-pressure pump ........................................................................................ 67
4.1.3 Eluents.............................................................................................................. 67
4.1.4 Peristaltic pump................................................................................................ 68
4.1.5 Suppressor module «MSM II» .......................................................................... 68
4.1.6 Connections ..................................................................................................... 69
4.2 Maintenance and servicing .......................................................................69
4.2.1 General information.......................................................................................... 69
4.2.2 Passivation ....................................................................................................... 70
4.2.3 Recycling.......................................................................................................... 70
4.2.4 Shutdown ......................................................................................................... 70
4.2.5 Changing separating columns......................................................................... 71
4.2.6 Maintenance work at the pump head .............................................................. 72
4.2.7 Regeneration of the suppressor module «MSM II».......................................... 76
4.2.8 Cleaning the suppressor.................................................................................. 77
4.2.9 Replacing the suppressor................................................................................ 79
4.2.10 Replacing the pump tubing ............................................................................. 80
4.3 Faults and malfunctions............................................................................82
4.3.1 Error messages ................................................................................................ 82
4.3.2 Malfunctions and their rectification .................................................................. 82
4.4 Diagnostic tests / Validation / GLP ...........................................................84
5 Appendix ................................................................... 85
5.1 Technical data............................................................................................85
II
861 Advanced Compact IC / Instructions for Use 8.861.1033
Table of contents
5.1.1 Conductivity measurement .............................................................................. 85
5.1.2 Conductivity detector ....................................................................................... 85
5.1.3 Injection valve ................................................................................................... 86
5.1.4 High-pressure pump ........................................................................................ 86
5.1.5 Peristaltic pump................................................................................................ 87
5.1.6 Suppressor module «MSM II» .......................................................................... 87
5.1.7 Leak detector.................................................................................................... 87
5.1.8 RS232 interface ................................................................................................ 87
5.1.9 Analog output ................................................................................................... 88
5.1.10 Remote interface .............................................................................................. 88
5.1.11 Mains connection ............................................................................................. 89
5.1.12 Safety specifications......................................................................................... 89
5.1.13 Electromagnetic compatibility (EMC)............................................................... 89
5.1.14 Ambient temperature........................................................................................ 89
5.1.15 Housing ............................................................................................................ 90
5.2 Standard equipment..................................................................................91
5.3 Optional accessories ................................................................................96
5.3.1 General accessories......................................................................................... 96
5.3.2 High-pressure pump ........................................................................................ 97
5.3.3 Separating columns and precolumns.............................................................. 98
5.3.4 Column heating .............................................................................................. 100
5.3.5 Communication .............................................................................................. 101
5.4 Warranty and Conformity........................................................................102
5.4.1 Warranty.......................................................................................................... 102
5.4.2 Declaration of Conformity............................................................................... 103
5.4.3 Quality Management Principles .....................................................................104
5.5 Index.........................................................................................................105
861 Advanced Compact IC / Instructions for Use 8.861.1033
III
Table of contents
List of figures
Figure 1: Front 861 Advanced Compact IC.............................................................. 3
Figure 2: Rear panel 861 Advanced Compact IC..................................................... 4
Figure 3: Interior of the IC 2.861.0010 (with permanently attached accessories
and 1.733.0110 Detector block)................................................................ 5
Figure 4: Interior of the IC 2.861.0020 (with permanently attached accessories,
suppressor module «MSM II» and 1.733.0110 Detector block) ................ 7
Figure 5: Interior of the IC 2.861.0040 (with permanently attached accessories,
1.733.0110 Detector block, suppressor module «MSM II» and 853 CO
Suppressor)............................................................................................... 9
Figure 6: Connecting diagram for 2.861.0010 Compact IC without suppressor ... 15
Figure 7: Connecting diagram for 2.861.0020 Compact IC with suppressor
module «MSM II» 46 ................................................................................ 15
Figure 8: Connecting diagram for 2.861.0040 Compact IC with suppressor
module «MSM II» 46 and 853 CO
Suppressor MCS 53......................... 16
2
Figure 9: Connectors for capillaries........................................................................ 19
Figure 10: 6.2821.120 Filter unit PEEK ..................................................................... 20
Figure 11: Setting the mains voltage........................................................................ 22
Figure 12: Connection of the pulsation dampener................................................... 26
Figure 13: Connection of eluent bottle ..................................................................... 28
Figure 14: Installation of column without suppressor............................................... 33
Figure 15: Installing pump tubings ........................................................................... 36
Figure 16: Connection of separation column with suppressor module «MSM II» .... 37
Figure 17: Connection of supply bottles................................................................... 40
Figure 18: Connections at suppressor module «MSM II»........................................ 41
Figure 19: Components of the pump head .............................................................. 73
Figure 20: Replacement of the piston seal 98.......................................................... 74
Figure 21: Components of inlet valve 99 and outlet valve 100 ............................... 76
Figure 22: Assembling the suppressor .................................................................... 78
2
IV
861 Advanced Compact IC / Instructions for Use 8.861.1033
Table of contents
List of numbered parts and controls
1 Door to interior
35 Connection capillary
2 Connection purge valve
3 Connection for syringe
4 Feedthrough
5 Pilot lamp
6 Bottle rack
7 Opening
8 Opening
9 Connection for drain tube
10 Opening
11 Opening
12 Opening for detector cable
13 Knurled screw
14 Detachable rear panel
15 Transport security screws
16 Mains switch
17 Mains connection plug
36 Connection capillary
37 Purge valve
38 Aspirating capillary
39 Connection capillary
40 Pump head
41 Mounting rail
42 Fastening screws
43 Connection capillary
44 Inlet capillary for detector block
45 Detector block
46 Suppressor module «MSM II»
47 Tubing cartridge
48 Contact pressure lever
49 Holding clamp
50 Snap-action lever
51 Pump drive
18 Fuse holder
19 Serial number
20 Analog output
21 Remote interface
22 Connection for detector block
23 RS232 interface
24 Inlet capillary for injection valve
25 Mounting rail
26 Column connection capillary
27 Sample loop
28 Injection valve
29 Aspirating tubing
30 Connection capillary to syringe
31 PEEK coupling
32 Leak detector
33 Connection capillary
52 Mounting pin
53 853 CO
Suppressor
2
54 Compression fitting
55 Compression fitting
56 Capillary
57 Filter-Screw of Filter Unit
58 Filter
59 Filter-Housing of Filter Unit
60 Pulsation dampener
61 Connection to injection valve
62 Connection to purge valve
63 Aspirating tubing
64 Tubing nipple
65 Threaded stopper
66 Bottle attachment
67 Eluent bottle
34 Filter unit PEEK
861 Advanced Compact IC / Instructions for Use 8.861.1033
68 Aspirating filter
V
Table of contents
69 CO2 absorber
70 Cotton wool
71 SGJ clip
72 Absorber tube
73 Separating column
74 Column holder
75 Aspirating tubing for H
76 Aspirating tubing for H
O
2
2SO4
77 Coupling
78 Pump tubing (6.1826.110) for H
79 Pump tubing (6.1826.110) for H
2SO4
O
2
80 Stopper (orange-yellow)
81 PEEK Coupling with filter and tubing
security device
82 Suppressor inlet capillary for eluent
83 Suppressor outlet capillary for eluent
105 Sealing ring
106 Sleeve
107 Sapphire sleeve
108 Sapphire sphere
109 Ceramic holder for sapphire sphere
110 Seal
111 Screw nut
112 Connection piece
113 Suppressor rotor
114 Suppressor holder
115 Slot in the suppressor holder
84 Suppressor inlet capillary for H
85 Suppressor inlet capillary for H
86 Suppressor outlet capillary for H
87 Suppressor outlet capillary for H
88 Bottle attachment
89 Supply bottle
90 Screw for piston cartridge
91 Zircon piston
92 Spring retainer
93 Spring
94 Piston cartridge
95 Piston guide sleeve
96 Sapphire supporting ring
97 Sapphire supporting ring
98 Piston seal
99 Inlet valve
O
2
2SO4
O
2
2SO4
100 Outlet valve
101 Screw holder
102 Special tool
103 Special tool
104 Valve housing
VI
861 Advanced Compact IC / Instructions for Use 8.861.1033
1.1 Instrument description
1 Introduction
1.1 Instrument description
The 861 Advanced Compact IC is a PC-controlled system for ion
chromatographic analyses. The three following versions are available:
• 2.861.0010 without suppressor
• 2.861.0020 with suppressor module «MSM II»
• 2.861.0040 with suppressor module «MSM II»
and 853 CO
The extremely compact housing of the 861 Advanced Compact IC contains everything needed to carry out ion chromatography at the highest
quality level:
• Injection valve – for individual injections or for use with a sample
changer such as the Metrohm 838 Advanced Sample Processor
Suppressor (MCS)
2
• High-pressure pump – extremely low-pulsation double piston
pump with a flow range from 0.2 … 2.5 mL/min and a maximum
pressure of 35 MPa (350 bar)
• Pulsation dampener – even with low-level pressure variations the
pulsation dampener reliably protects the column against damage
• Column chamber – the perfect insulation of the housing provides
not only thermally stable conditions for the separation column but
also shields the system against electromagnetic interference
• Columns – whether anion columns with or without suppression,
separation columns for cations or organic acids – the 861 Advanced Compact IC can accommodate them all
• Suppressor module – the Metrohm suppressor module (MSM) is
already integrated in the versions 2.861.0020 and 2.861.0040 –
pressure-resistant, with fully automatic regeneration, highest performance and optimal reproducibility
• Peristaltic pump – integrated two-channel peristaltic pump with a
flow rate of 0.4 … 0.5 mL/min for regeneration and rinsing of the
suppressor module «MSM II» built into the versions 2.861.0020 and
2.861.0040.
• Detector – conductivity detector with outstanding temperature
stability. The detector temperature varies by less than 0.01°C and
can be optimally adapted to the ambient conditions.
• 853 CO
pressor (MCS) is built in downline from the suppressor module
«MSM II». The·853 CO
the eluent. This reduces the background conductivity, improves detection sensitivity and minimizes the injection and carbonate peak.
861 Advanced Compact IC / Instructions for Use 8.861.1033
Suppressor – in Version 2.861.0040 the 853 CO2 Sup-
2
Suppressor (MCS) removes the CO2 from
2
1
1 Introduction
All components which come into contact with eluent and sample
are metal-free.
The operation of the 861 Advanced Compact IC takes place via a PC
connected to the RS232 interface with the help of the «IC Net» control
and evaluation program. This PC program can be used to create systems for recording and evaluating chromatograms. Time programs can
also be created in which a large number of instrument functions can be
triggered for each program step. It is also possible to use programmable signals to control external instruments via the remote interface.
The «IC Net» operating software meets all the requirements you could
place today on a modern integration software: single or multi-point calibration, internal or external standard, selectable algorithms for non-linear calibration, various integration modes with integration parameters
and integration events, different methods for peak recognition, peak
editor, free scaling, superimposing several chromatograms, use of
sample tables and batch reprocessing; a powerful and GLP-conform
report generator with output interfaces for monitor, printer and external
databases.
The independent «Autodatabase» PC program supplied can be used to
save and handle results and chromatograms produced by the «IC Net»
program in a database. With «Autodatabase» data can be sorted, filtered and searched with the help of different criteria. In addition, data
and curves can be printed out according to user-defined report templates.
The «IC Net» software can be configured and used in order to comply
with the Electronic Records and Signatures Rule, known as 21 CFR
Part 11, established by the U.S. Food and Drug Administration (FDA).
For this purpose the program contains password protection, user administration, electronic signatures, audit trail and administration of methods and results in databases. To use the 21 CFR Part 11 features of
«IC Net» the operating system Windows 2000 or Windows XP with
NTFS file system is required.
2
861 Advanced Compact IC / Instructions for Use 8.861.1033
1.2 Parts and controls
1.2 Parts and controls
In this Section you will find the numbers and designations of the parts
and controls of the 861 Advanced Compact IC. The numbering applies throughout the Instructions for Use, i.e. bold numbers in the text
3
(e.g.
1.2.1 Front
6
) refer to the parts and controls illustrated here.
1
5
Figure 1: Front 861 Advanced Compact IC
Door to inner compartment
1
Connection purge valve
2
Connection for 6.2816.020 syringe
3
for aspiration of the sample
Feedthrough
4
for capillaries
2
3
4
Pilot lamp
5
is on when the instrument is switched
on
Bottle rack
6
for holding supply bottles with eluent,
regeneration solution, and rinsing solution
861 Advanced Compact IC / Instructions for Use 8.861.1033
3
1 Introduction
1.2.2 Rear panel
12
13
19
20
21
7
8
9
10
11
13
14
15
16
17
18
22
Figure 2: Rear panel 861 Advanced Compact IC
Opening
7
for in- and outlets
Opening
8
for in- and outlets
Connection for drain tube
9
for discharge of spilled liquid from the
bottle rack
Opening
10
for in- and outlets
Opening
11
for in- and outlets
Opening for detector cable
12
Knurled screw
13
for fastening the rear panel
23
Detachable rear panel
14
Access to the inner compartment
Transport security screws
15
to secure the pump head when the instrument is transported
Mains switch
16
to switch instrument on and off:
I = ON 0 = OFF
Mains connection plug
17
Mains connection, see Section 2.4
Fuse holder
18
Changing the fuses, see Section 2.4.2
Serial number
19
Analog output
20
output for analogue signal
4
861 Advanced Compact IC / Instructions for Use 8.861.1033
1.2 Parts and controls
Remote interface
21
Remote-I/O lines for connection of external devices
Connection for detector block
22
1.2.3 Interior 2.861.0010
45
44
41
RS232 interface
23
PC connection
1
24
25
26
27
43
42
41
40
39
38
37
36
28
25
29
30
3435
313233
Figure 3: Interior of the IC 2.861.0010 (with permanently attached accesso-
ries and 1.733.0110 Detector block)
861 Advanced Compact IC / Instructions for Use 8.861.1033
5
1 Introduction
1 Door to inner compartment
Inlet capillary for injection valve
24
PEEK capillary 6.1831.010,
length L = 24 cm
Mounting rail
25
for 6.2027.0X0 column holder
Column connection capillary
26
6.1831.010 PEEK capillary,
length L = 30 cm
Sample loop
27
20 µL PEEK sample loop 6.1825.210
Injection valve
28
Aspirating tubing
29
for sample;
PTFE-tubing 6.1803.020,
length L = 52 cm
Connection capillary
35
6.1831.010 PEEK capillary,
length L = 13 cm
Connection capillary
36
6.1831.010 PEEK capillary,
length L = 15 cm
Purge valve
37
Aspirating capillary
38
Connection for 6.1834.010 aspirating
tubing
Connection capillary
39
Connection pump head – purge
valve, fixed mounting
Pump head (6.2824.100)
40
Mounting rail
41
for cartridge holder
Connection capillary to syringe
30
6.1803.020 PTFE tubing,
length L = 30 cm
PEEK coupling (6.2744.040)
31
Leak detector
32
Connection capillary
33
6.1831.010 PEEK capillary,
length L = 13 cm
Filter unit PEEK (6.2821.120)
34
Fastening screws
42
for pump head 40
Connection capillary
43
in pump head, fixed mounting
Inlet capillary for detector block
44
PEEK capillary, fixed mounting
Detector block (1.732.0110)
45
6
861 Advanced Compact IC / Instructions for Use 8.861.1033
1.2 Parts and controls
1.2.4 Interior 2.861.0020
1
24
25
45
44
41
26
27
28
43
42
41
40
39
38
37
36
35
46
25
30
29
47
48
49
323334
31
52
51
50
Figure 4: Interior of the IC 2.861.0020 (with permanently attached accesso-
ries, suppressor module «MSM II» and 1.733.0110 Detector
block)
1 Door to inner compartment
24 Inlet capillary for injection valve
PEEK capillary 6.1831.010,
length L = 24 cm
861 Advanced Compact IC / Instructions for Use 8.861.1033
25 Mounting rail
for 6.2027.0X0 column holder
26 Column connection capillary
6.1831.010 PEEK capillary,
length L = 30 cm
7
1 Introduction
27 Sample loop
20 µL PEEK sample loop 6.1825.210
28 Injection valve
29 Aspirating tubing
for sample;
PTFE-tubing 6.1803.020,
length L = 52 cm
30 Connection capillary to syringe
6.1803.020 PTFE tubing,
length L = 30 cm
31 PEEK coupling (6.2744.040)
32 Leak detector
33 Connection capillary
6.1831.010 PEEK capillary,
length L = 13 cm
34 Filter unit PEEK (6.2821.120)
41 Mounting rail
for cartridge holder
42 Fastening screws
for pump head 40
43 Connection capillary
in pump head, fixed mounting
44 Inlet capillary for detector block
PEEK capillary, fixed mounting
45 Detector block (1.732.0110)
Suppressor module «MSM II»
46
(inlet and outlet capillaries are not
shown)
Tubing cartridge (6.2755.000)
47
for 6.1826.110 pump tubing
Contact pressure lever
48
for adjusting the contact pressure
35 Connection capillary
6.1831.010 PEEK capillary,
length L = 13 cm
36 Connection capillary
6.1831.010 PEEK capillary,
length L = 15 cm
37 Purge valve
38 Aspirating capillary
Connection for 6.1834.010 aspirating
tubing
39 Connection capillary
Connection pump head – purge
valve, fixed mounting
40 Pump head (6.2824.100)
Holding clamp
49
for locking the tubing cartridge into
place
Snap-action lever
50
for releasing the tubing cartridge
Pump drive
51
roller head with contact rollers
Mounting pin
52
for attaching the tubing cartridges
8
861 Advanced Compact IC / Instructions for Use 8.861.1033
1.2 Parts and controls
1.2.5 Interior 2.861.0040
45
44
1
24
25
53
41
43
42
41
40
39
38
37
36
26
27
28
46
25
30
29
47
48
49
35
Figure 5: Interior of the IC 2.861.0040 (with permanently attached accesso-
ries, 1.733.0110 Detector block, suppressor module «MSM II» and
853 CO
Suppressor)
2
1 Door to inner compartment
24 Inlet capillary for injection valve
PEEK capillary 6.1831.010,
length L = 24 cm
861 Advanced Compact IC / Instructions for Use 8.861.1033
323334
31
52
51
50
25 Mounting rail
for 6.2027.0X0 column holder
26 Column connection capillary
6.1831.010 PEEK capillary,
length L = 30 cm
9
1 Introduction
27 Sample loop
20 µL PEEK sample loop 6.1825.210
28 Injection valve
29 Aspirating tubing
for sample;
PTFE-tubing 6.1803.020,
length L = 52 cm
30 Connection capillary to syringe
6.1803.020 PTFE tubing,
length L = 30 cm
31 PEEK coupling (6.2744.040)
32 Leak detector
33 Connection capillary
6.1831.010 PEEK capillary,
length L = 13 cm
34 Filter unit PEEK (6.2821.120)
41 Mounting rail
for cartridge holder
42 Fastening screws
for pump head 40
43 Connection capillary
in pump head, fixed mounting
44 Inlet capillary for detector block
PEEK capillary, fixed mounting
45 Detector block (1.732.0110)
46 Suppressor module «MSM II»
(inlet and outlet capillaries are not
shown)
47 Tubing cartridge (6.2755.000)
for 6.1826.110 pump tubing
48 Contact pressure lever
for adjusting the contact pressure
35 Connection capillary
6.1831.010 PEEK capillary,
length L = 13 cm
36 Connection capillary
6.1831.010 PEEK capillary,
length L = 15 cm
37 Purge valve
38 Aspirating capillary
Connection for 6.1834.010 aspirating
tubing
39 Connection capillary
Connection pump head – purge
valve, fixed mounting
40 Pump head (6.2824.100)
49 Holding clamp
for locking the tubing cartridge into
place
50 Snap-action lever
for releasing the tubing cartridge
51 Pump drive
roller head with contact rollers
52 Mounting pin
for attaching the tubing cartridges
53
853 CO
Suppressor
2
(inlet and outlet capillaries are not
shown)
10
861 Advanced Compact IC / Instructions for Use 8.861.1033
1.3 Information on the Instructions for Use
1.3 Information on the Instructions for Use
Please read through these Instructions for Use carefully before you put
the 861 Advanced Compact IC into operation. The Instructions for Use
contain information and warnings to which the user must pay attention
in order to assure safe operation of the instrument.
1.3.1 Organization
These Instructions for Use 8.861.1033 for the 861 Advanced Compact IC provide a comprehensive overview of installation, startup procedure, operation, fault rectification and technical specifications of this
instrument. The Instructions for Use are organized as follows:
Sect. 1 Introduction
General description of instrument, parts and controls and
safety notes
Sect. 2 Installation
Installation of instrument, accessories,
and external devices
Sect. 3 Operation
Introduction to the operation using an example
Sect. 4 Notes - Maintenance - Faults
Notes on ion chromatography, maintenance, fault rectification, diagnostic tests, validation
Sect. 5 Appendix
Technical data, standard equipment, options, warranty,
declarations of conformity, index
To find the required information on the instruments, use either the Ta-
ble of contents or the Index at the back.
As a supplement to the Instructions for Use, the Metrohm Monograph
8.792.5003 "Practical Ion Chromatography" is also supplied. This
provides an introduction to the theoretical fundamentals and general information about determinations.
861 Advanced Compact IC / Instructions for Use 8.861.1033
11
1 Introduction
1.3.2 Notation and pictograms
The following notations and pictograms (symbols) are used in these Instructions for Use:
Fill Menu item, parameter or entry
value
in the software
SYSTEM STATE Program window
in the software
<OK> Button
in the software
22 Part or control of 861
Hazard
This symbol draws attention to a
possible danger to life or of injury if
the associated directions are not
followed correctly.
Warning
This symbol draws attention to possible damage to instruments or instrument parts if the associated directions are not followed correctly.
Caution
This symbol marks important information. First read the associated directions before you continue.
Comment
This symbol marks additional information and tips.
12
861 Advanced Compact IC / Instructions for Use 8.861.1033
1.4 Safety notes
1.4 Safety notes
1.4.1 Electrical safety
While electrical safety in the handling of the 861 Advanced Compact IC
is assured in the context of the specifications EN / IEC 61010-1 (protection class
noted:
• Mains connection
Setting of the mains voltage, checking the mains fuse and the
mains connection must be effected in accordance with the instruc-
tions in Section 2.4.
• Opening the 861 Advanced Compact IC
If the 861 Advanced Compact IC is connected to the power supply,
the instrument must not be opened nor must parts be removed from it,
otherwise there is a danger of coming into contact with components
which are live. Therefore always disconnect the instrument from all
voltage sources before you open it and ensure that the mains cable
is disconnected from mains connection
I, degree of protection IP20), the following points should be
17
!
• Protection against static charges
Electronic components are sensitive to static charging and can be
destroyed by discharges. Before you touch any of the components inside the 861 Advanced Compact IC, you should ground yourself and
any tools you are using by touching a grounded object (e.g. housing
of the instrument or a radiator) to eliminate any static charges which
exist.
1.4.2 General precautionary rules
• Handling of solvents
Check all lines of the IC system periodically for possible leaks. Follow
the relevant instructions regarding the handling of flammable and/or
toxic solvents and their disposal.
861 Advanced Compact IC / Instructions for Use 8.861.1033
13
2 Installation
2 Installation
2.1 Overview
2.1.1 Flow chart
The following flow chart provides an overview of all installation work.
You will find more detailed information in the relevant Sections.
Setting up sect. 2.2
Installing accessories
Mains connection
Connecting PC sect. 2.5
Connecting high press. pump sect. 2.6
Precolumn
No
Choosing sample loop sect. 2.7.3
Connecting column sect. 2.7.4/5
Suppressor module
(MSM II)?
No
sect. 2.3
sect. 2.4
Yes
Connecting precolumn sect. 2.7.1
Yes
Connecting suppressor module (MSM II) sect. 2.8
853 CO
2
Suppressor?
No
Yes
Connecting 853 CO2 Suppressor sect. 2.9
Conditioning sect. 2.10
Connecting extern al devices sect. 2.11
2.1.2 Connections in the 861 Advanced Compact IC
The two following illustrations show the internal connections in the 861
Advanced Compact IC in schematic form. The meanings of the various
numbered components are given in the detailed illustrations and descriptions in Sections 2.2 – 2.11.
14
861 Advanced Compact IC / Instructions for Use 8.861.1033
2.1 Overview
66
67
68
63
40
38
43
35
37
Eluent
36
39
34
60
24
33
30
27
26
28
Injection valve
29
Sample
73
Column
44
45
Detector
Waste
66
67
63
Figure 6: Connecting diagram for 2.861.0010 Compact IC without suppres-
sor
45
31
44
Detector
39
27
28
26
73
82
83
43
40
38
34
24
33
85
87
46
84
86
35
37
78
36
60
30
29
76
77
88
81
79
75
89
68
Eluent
Figure 7: Connecting diagram for 2.861.0020 Compact IC with suppressor
module «MSM II»
861 Advanced Compact IC / Instructions for Use 8.861.1033
Sample
46
H
2SO4
H2O
Waste
15
2 Installation
66
67
68
63
38
40
43
35
37
Eluent
36
39
34
24
33
27
28
26
85
73
87
82
83
46
53
84
44
Detector
86
45
78
60
30
29
76
77
88
81
79
75
89
Sample
H
2SO4
H2O
Waste
Figure 8: Connecting diagram for 2.861.0040 Compact IC with suppressor
module «MSM II»
46
and 853 CO2 Suppressor MCS 53.
2.2 Setting up the instrument
2.2.1 Packaging
The 861 Advanced Compact IC is supplied together with the separately
packed accessories in special packagings containing shock-absorbing
foam linings designed to provide excellent protection. The instrument
itself is packed in an evacuated polyethylene bag to prevent the ingress
of dust. Please store all these special packagings as only they assure
transport of the instrument free from damage.
2.2.2 Check
After receipt, immediately check whether the shipment is complete and
has arrived without damage (compare with delivery note and list of
accessories in Section 5.2). In the case of transport damage, see instructions in Section 5.4.1 "Warranty".
2.2.3 Location
Position the instrument in the laboratory at a location convenient for operation, free from vibrations and protected against a corrosive atmosphere and contamination by chemicals.
16
861 Advanced Compact IC / Instructions for Use 8.861.1033
2.3 Attaching the accessories
To avoid disturbing temperature influences on the insulated column
compartment, the instrument must be protected against direct sunlight.
2.3 Attaching the accessories
2.3.1 Connection of detector block
The metal-free 1.732.0110 Detector block belongs to the scope of
supply of the 861 Advanced Compact IC; it must be inserted in the instrument and connected up. Proceed as follows:
If the detector block needs to be replaced then the cell constant of
the new one must be entered. On the rear of the detector block the
cell constant measured in the factory is printed on: c = XX.X /cm. This
value should be entered in the software (see Cap. 3.3.2) in order to
ensure that the conductivity is displayed accurately.
1 Install detector block
• Unscrew the four knurled screws 13 from the top rear panel
14 of the 861 Advanced Compact IC and remove rear panel
(see Figure 2)
• Position detector block 45 from the back in the space pro-
vided in the 861 Advanced Compact IC and push fully to the
front (see Figure 3, Figure 4 and Figure 5).
• Insert the cable permanently attached to the detector block
45 in one of the openings 12 and the outlet capillary in one of
the openings 8 of the rear panel 14.
You can now place the 853 CO
tector block of Version 2.861.0040 so that you do not have to
Suppressor beside the de-
2
remove the rear panel again (see Figure 5). Connecting the
853 is described in detail in Section 2.9. Pull the Remote cable and the mains cable out of opening 11 in the rear panel.
2 Replace rear panel
• Replace rear panel 14 and screw onto the 861 Advanced
Compact IC using the four knurled screws 13.
3 Connect detector block
• Plug the gray connecting cable permanently attached to the
detector block 45 into connection 22 "Detector Block" of the
861 Advanced Compact IC and fasten to the instrument by
tightening the screws in the cable connector (see Figure 2).
4 Connect waste container
• Lead the outlet capillary of the detector block 45 to a suffi-
ciently large waste container and fix in place.
861 Advanced Compact IC / Instructions for Use 8.861.1033
17
2 Installation
2.3.2 Connection of syringe and aspirating tubing
For manual filling of the sample loops 27 mounted on the injection
valves, the 6.2816.020 Syringe and the PTFE aspirating tubing 29 already screwed to the valve are needed. These accessories are
mounted or adjusted as follows:
1 Connect syringe
• Remove the plastic stopper from connection socket 3 on the
front side of the 861 Advanced Compact IC (see Figure 1).
• Push 6.2816.020 Syringe (without needle) as far as it will go
into connection socket 3.
2 Lead aspirating tubing to the outside
• Lead the PTFE aspirating tubing 29 connected to the injec-
tion valve 28 through one of the feedthroughs 4 to the outside.
2.3.3 Connection of the drain tube for the inner compartment
The 861 Advanced Compact IC has a connection at the front to which a
drain tube for discharged liquids in the inner compartment can be attached. Proceed as follows:
1 Connect drain tube
• Mount 6.1816.020 Silicone tubing on connection nipple on
the lower right side.
2 Lead drain tube to collecting vessel
• Lead the other end of the drain tube to a suitable collecting
vessel and fix in place.
2.3.4 Connection of the drain tube for bottle rack
The 861 Advanced Compact IC has a connection at the rear to which a
drain tube for discharged liquids in the bottle rack can be attached.
Proceed as follows:
1 Connect drain tube
• Mount 6.1816.020 Silicone tubing on connection nipple 9
(see Figure 2).
2 Lead drain tube to collecting vessel
• Lead the other end of the drain tube to a suitable collecting
vessel and fix in place.
2.3.5 Connection of PEEK capillaries
For the connections between high-pressure pump and detector block
6.1831.010 PEEK capillaries (i.d. = 0.25 mm, o.d. =
which are connected using either 6.2744.010 PEEK compression fit-
tings (long) or 6.2744.070 PEEK compression fittings (short).
18
861 Advanced Compact IC / Instructions for Use 8.861.1033
1
/16") are used
2.3 Attaching the accessories
These PEEK connectors can also be used to connect 6.1822.010 PTFE
microcapillaries (i.d. = 0.3 mm). Proceed as follows:
Capillaries fitted with new connectors must have a perfectly flat cut
surface. To cut PEEK or PTFE capillaries it is best to use the
6.2621.080 Capillary tubing cutter.
1 Mount compression fitting
• Slide a compression fitting 54 (6.2744.010) or a compression
fitting 55 (6.2744.070) over the end of the capillary 56 to be
fastened as shown in Figure 9.
2 Insert capillary in connection
• Push capillary end in the corresponding connection as far as
it will go (to avoid dead volume).
3 Tighten compression fitting
• Tighten compression fitting 54 or 55 by hand (never use
tools).
54
56
Figure 9: Connectors for capillaries
2.3.6 Filter unit PEEK
One 6.2821.120 Filter unit PEEK (see Figure 10) is installed between
the high-pressure pump and injection valve 28. This filter unit serves to
avoid contamination by abrasive particles of the piston seals.
The Filter unit PEEK 34 consists of the filter-housing 59, the filter-screw
57 and the 6.2821.130 Filter 58. For the connection of capillaries 56
PEEK compression fittings 54/55 (6.2744.010 or 6.2744.070) must be
used. New filters 58 are available as an option with the ordering number
6.2821.130 (set of 10).
When connecting the filter unit please note the flow direction arrow
printed on the housing.
55
Compression fitting
54
(6.2744.010)
Compression fitting
55
(6.2744.070)
Capillary
56
6.1831.010 PEEK capillary or
6.1822.010 PTFE microcapillary
861 Advanced Compact IC / Instructions for Use 8.861.1033
19
2 Installation
34
56
54 57
Figure 10: 6.2821.120 Filter unit PEEK
34 Filter unit PEEK (6.2821.120)
54 Compression fitting (6.2744.010)
56 Capillary
6.1831.010 PEEK capillary or 6.1822.010
PTFE microcapillary
58
59
Filter screw of filter unit
57
54
Part of 6.2821.120 Filter unit
6.2821.130 Filter
58
Filter housing of filter unit
59
Part of 6.2821.120 Filter unit
56
20
861 Advanced Compact IC / Instructions for Use 8.861.1033
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