Metrohm 761 User Manual
761 Compact IC
METROHM Ltd.
CH-9101 Herisau
Switzerland
Phone ++41 71 353 85 85
Fax ++41 71 353 89 01
8.761.1063
Instructions for Use
CH-9101 Herisau/Switzerland
Phone ++41 71 353 85 85
Fax ++41 71 353 89 01
Internet www.metrohm.ch
E-Mail info@metrohm.ch
761 Compact IC
Program «761 PC Software 1.1»
8.761.1063 Instructions for Use
07.07.2004 / chs
Table of contents
Table of contents
1 Introduction............................................................................................................1
1.1 Instrument description .......................................................................................... 1
1.2 Parts and controls .................................................................................................. 3
1.3 Information on the Instructions for Use ...........................................................10
1.3.1 Organization ......................................................................................... 10
1.3.2 Notation and pictograms...................................................................... 11
1.4 Safety notes........................................................................................................... 12
1.4.1 Electrical safety..................................................................................... 12
1.4.2 General precautionary rules ................................................................. 12
2 Installation .......................................................................................................... 13
2.1 Overview ................................................................................................................13
2.1.1 Flow chart ............................................................................................. 13
2.1.2 Connections in the 761 Compact IC.................................................... 13
2.2 Setting up the instrument.................................................................................... 15
2.2.1 Packaging............................................................................................. 15
2.2.2 Check.................................................................................................... 15
2.2.3 Location ................................................................................................ 15
2.3 Attaching the accessories ..................................................................................15
2.3.1 Connection of detector block............................................................... 15
2.3.2 Connection of syringe and aspirating tubing ....................................... 16
2.3.3 Connection of the drain tube for the inner compartment..................... 16
2.3.4 Connection of the drain tube for bottle rack ........................................ 17
2.3.5 Connection of PEEK capillaries............................................................ 17
2.3.6 Filter unit PEEK ..................................................................................... 18
2.4 Mains connection .................................................................................................19
2.4.1 Setting the mains voltage..................................................................... 19
2.4.2 Fuses .................................................................................................... 20
2.4.3 Mains cable and mains connection ..................................................... 20
2.4.4 On/off switching of the instrument ....................................................... 20
2.5 Connection to the PC........................................................................................... 21
2.5.1 Connecting cable ................................................................................. 21
2.5.2 Software installation.............................................................................. 21
2.5.3 Basic settings ....................................................................................... 22
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 ................................................................ 27
2.6.4 Deaerating the pump and rinsing the pulsation dampener................. 29
761 Compact IC
2.7 Precolumns and separating columns ............................................................... 31
2.7.1 General information on precolumns..................................................... 31
2.7.2 Precolumns with cartridge head........................................................... 31
2.7.3 Precolumn glass cartridges with cartridge holder ............................... 33
2.7.4 IC anion precolumn SUPERSEP .......................................................... 34
2.7.5 General information on separating columns........................................ 35
2.7.6 Selection of the sample loop................................................................ 35
2.7.7 Installation of the separating column without suppressor ................... 36
2.7.8 Installation of the separating column with suppressor ........................ 37
I
Table of contents
2.8 Suppressor module ............................................................................................. 38
2.8.1 General information on suppressor module........................................ 38
2.8.2 Preparation of the peristaltic pump...................................................... 38
2.8.3 Connection of supply bottles ............................................................... 41
2.8.4 Connection of the suppressor module ................................................ 43
2.9 Putting into operation.......................................................................................... 45
2.9.1 Putting into operation without suppressor ........................................... 45
2.9.2 Putting into operation with suppressor ................................................ 46
2.10 Connection of external devices ......................................................................... 49
2.10.1 Connection of the 750 Autosampler .................................................... 49
2.10.2 Connection of the 766 IC Sample Processor ...................................... 50
2.10.3 Connection of other devices ................................................................ 52
3 Operating tutorial ....................................................................................... 53
3.1 Requirements........................................................................................................ 53
3.2 Preparations.......................................................................................................... 54
3.3 Calibration ............................................................................................................. 55
3.4 Sample determination ......................................................................................... 63
4 Operation............................................................................................................... 67
4.1 Fundamentals of the operation.......................................................................... 67
4.1.1 Starting/closing the program ............................................................... 67
4.1.2 Glossary................................................................................................ 68
4.1.3 Overview of program windows............................................................. 69
4.1.4 Main window elements......................................................................... 70
4.1.5 Icons of the main window..................................................................... 70
4.1.6 Overview of file types............................................................................ 71
4.1.7 Context sensitive menus ...................................................................... 72
4.1.8 Keyboard and mouse functions........................................................... 72
4.1.9 Help ...................................................................................................... 73
4.2 Instrument and software settings...................................................................... 74
4.2.1 Fonts..................................................................................................... 74
4.2.2 Security system .................................................................................... 74
4.2.3 Global settings ..................................................................................... 75
4.2.4 COM port.............................................................................................. 77
4.3 Systems ................................................................................................................. 78
4.3.1 System window .................................................................................... 78
4.3.2 System file handling ............................................................................. 78
4.3.3 System functions .................................................................................. 79
Connect and disconnect system ................................................. 79
Start/stop hardware and record baseline .................................... 79
Start/stop determinations............................................................. 80
Options for determinations........................................................... 80
4.3.4 System settings .................................................................................... 82
Modify system window ................................................................. 82
Watch window display.................................................................. 82
Set start mode .............................................................................. 82
Print system parameters .............................................................. 83
4.3.5 PC icon ................................................................................................. 83
761 Compact IC
II
Table of contents
Menu options for PC icon............................................................. 83
Select processing method and data source................................ 83
4.3.6 Watch window....................................................................................... 84
Menu options for screen icon....................................................... 84
4.3.7 Instrument icon ..................................................................................... 85
Menu options for instrument icon................................................. 85
System parameters for disconnected system ............................. 85
Instrument control for connected system .................................... 86
Time program ............................................................................... 88
Configuration ................................................................................90
Hardware settings ........................................................................ 91
4.3.8 Timer .....................................................................................................94
4.3.9 System state window............................................................................ 95
Status messages.......................................................................... 95
Error messages ............................................................................ 96
4.4 Methods .................................................................................................................97
4.4.1 Method file handling ............................................................................. 97
4.4.2 Passport................................................................................................ 97
General ......................................................................................... 98
Sample.......................................................................................... 99
Column ....................................................................................... 100
Eluent .......................................................................................... 101
Comment .................................................................................... 101
Method Log ................................................................................ 102
Data Log ..................................................................................... 103
4.4.3 Method setup...................................................................................... 104
General ....................................................................................... 104
Measure ...................................................................................... 104
Filters .......................................................................................... 105
Processing.................................................................................. 106
Math ............................................................................................ 107
4.4.4 Integration........................................................................................... 109
Setup........................................................................................... 110
Events ......................................................................................... 112
4.4.5 Calibration and quantification............................................................. 117
General information .................................................................... 117
Notations..................................................................................... 118
External standard calibration...................................................... 119
Component table........................................................................ 119
Peak identification ...................................................................... 121
Concentration table .................................................................... 123
Calibration curve......................................................................... 125
Update calibration ...................................................................... 127
Load and save calibration data.................................................. 128
Import and export calibration data ............................................. 128
Put out calibration curves ........................................................... 128
4.4.6 Report output...................................................................................... 129
Report options ............................................................................129
4.5 Chromatograms..................................................................................................141
4.5.1 Chromatogram window ...................................................................... 141
4.5.2 Chromatogram file handling............................................................... 142
Open chromatogram.................................................................. 142
Save chromatogram................................................................... 143
Close chromatogram.................................................................. 143
Delete chromatogram................................................................. 143
Export chromatogram................................................................. 143
Import chromatogram ................................................................ 144
4.5.3 Graphical representation.................................................................... 145
761 Compact IC
III
Table of contents
Appearance................................................................................ 145
Other graphical functions........................................................... 149
4.5.4 Peak editor.......................................................................................... 150
Switching on/off the peak editor ................................................ 150
Peak editor functions.................................................................. 150
Moving the cursor....................................................................... 151
4.5.5 Printing................................................................................................ 152
Page layout for printing .............................................................. 152
Printer settings............................................................................ 153
Print preview ............................................................................... 153
Printing........................................................................................ 153
4.5.6 Miscellaneous functions..................................................................... 153
Reintegration .............................................................................. 153
Recalibration............................................................................... 153
Subtraction of a chromatogram................................................. 154
Data compression ...................................................................... 154
Invert chromatogram.................................................................. 154
Autodatabase options................................................................ 155
Indicate active Autodatabase program ..................................... 155
4.6 Sample queue ..................................................................................................... 156
4.6.1 Sample queue file handling................................................................ 156
Open sample queue................................................................... 156
Save sample queue.................................................................... 156
Delete sample queue ................................................................. 156
4.6.2 Sample queue control ........................................................................ 157
Sample queue overview table .................................................... 157
Start sample queue .................................................................... 158
Pause sample queue ................................................................. 159
Cancel last run............................................................................ 159
Reset sample queue .................................................................. 159
4.6.3 Sample queue editor.......................................................................... 159
Open queue editor window........................................................ 159
Sample queue editor functions .................................................. 161
Print sample queue .................................................................... 161
Close sample queue editor ........................................................ 161
4.7 Batch reprocessing............................................................................................ 162
4.7.1 Batch reprocessing queue file handling ............................................ 162
Open batch reprocessing queue ............................................... 162
Create new batch reprocessing queue...................................... 162
Save batch reprocessing queue ................................................ 162
4.7.2 Perform batch reprocessing............................................................... 163
Reprocess options window........................................................ 163
Merge chromatograms .............................................................. 166
4.7.3 Batch reprocessing queue editor....................................................... 167
Open batch reprocessing queue editor window ....................... 167
Batch reprocessing queue editor functions............................... 168
Print batch reprocessing queue................................................. 168
Close batch reprocessing queue editor .................................... 168
761 Compact IC
IV
Table of contents
5 Notes – Maintenance – Faults....................................................169
5.1 Practical notes on ion chromatography .........................................................169
5.1.1 Separating columns............................................................................ 169
5.1.2 High-pressure pump .......................................................................... 170
5.1.3 Eluents ................................................................................................ 171
5.1.4 Peristaltic pump.................................................................................. 171
5.1.5 Suppressor module ............................................................................ 172
5.1.6 Connections........................................................................................ 172
5.2 Maintenance and servicing...............................................................................173
5.2.1 General information ............................................................................ 173
5.2.2 Passivation.......................................................................................... 173
5.2.3 Recycling ............................................................................................ 174
5.2.4 Shutdown............................................................................................ 174
5.2.5 Changing separating columns........................................................... 174
5.2.6 Maintenance work at the pump head ................................................176
5.2.7 Regeneration of the suppressor module ...........................................180
5.2.8 Cleaning the suppressor .................................................................... 181
5.2.9 Replacing the suppressor .................................................................. 183
5.2.10 Exchanging the pump tubing ............................................................. 185
5.3 Faults and malfunctions....................................................................................186
5.3.1 Error messages ..................................................................................186
5.3.2 Malfunctions and their rectification..................................................... 186
5.4 Diagnostic tests / Validation / GLP..................................................................188
6 Appendix.............................................................................................................. 189
6.1 Technical data.....................................................................................................189
6.1.1 Conductivity measurement................................................................. 189
6.1.2 Conductivity detector.......................................................................... 189
6.1.3 Injection valve .....................................................................................190
6.1.4 High-pressure pump .......................................................................... 190
6.1.5 Peristaltic pump.................................................................................. 191
6.1.6 Suppressor module ............................................................................ 191
6.1.7 Leak detector...................................................................................... 191
6.1.8 RS232 interface .................................................................................. 191
6.1.9 Remote interface................................................................................. 192
6.1.10 Analog output .....................................................................................192
6.1.11 Mains connection ............................................................................... 192
6.1.12 Safety specifications........................................................................... 192
6.1.13 Electromagnetic compatibility (EMC)................................................. 193
6.1.14 Ambient temperature.......................................................................... 193
6.1.15 Housing............................................................................................... 193
6.2 Standard equipment...........................................................................................194
6.3 Optional accessories .........................................................................................198
6.3.1 Accessories for capillary connections................................................ 198
6.3.2 High-pressure pump .......................................................................... 199
6.3.3 Separating columns and precolumns................................................ 200
6.3.4 Additional devices and cables ........................................................... 205
761 Compact IC
6.4 Warranty and conformity...................................................................................206
6.4.1 Warranty.............................................................................................. 206
6.4.2 EU Declaration of conformity.............................................................. 207
6.4.3 Certificate of conformity and system validation ................................. 208
6.5 Index .....................................................................................................................209
V
Table of contents
List of figures
Fig. 1: Front of the 761 Compact IC .......................................................................... 3
Fig. 2
: Rear of the 761 Compact IC........................................................................... 4
Fig. 3
: Interior of the 2.761.0010 Compact IC ...........................................................6
Fig. 4
: Interior of the 2.761.0020 Compact IC ...........................................................8
Fig. 5
: Connecting diagram for 2.761.0010 Compact IC without suppressor........ 14
Fig. 6
: Connecting diagram for 2.761.0020 Compact IC with suppressor............. 14
Fig. 7
: Connectors for capillaries............................................................................. 17
Fig. 8
: 6.2821.000 Filter unit PEEK ..........................................................................18
: Setting the mains voltage .............................................................................20
Fig. 9
Fig. 10
: Connection of the pulsation dampener........................................................ 26
Fig. 11
: Connection of eluent bottle........................................................................... 28
Fig. 12
: Installation of precolumn cartridges with cartridge head............................. 32
Fig. 13
: Installation of precolumn glass cartridges with cartridge holder ................. 34
Fig. 14
: Installation of column without suppressor.................................................... 37
Fig. 15
: Installing pump tubings ................................................................................39
Fig. 16
: Connection of the separating column with suppressor ...............................40
Fig. 17
: Connection of supply bottles........................................................................ 42
: Connections at suppressor module ............................................................. 43
Fig. 18
Fig. 19
: Components of the pump head .................................................................177
: Replacement of the piston seal 112 ..........................................................177
Fig. 20
Fig. 21
: Components of inlet valve 113 and outlet valve 114................................. 179
Fig. 22
: Assembling the suppressor........................................................................ 183
761 Compact IC
VI
Table of contents
List of numbered parts and controls
1 Door to interior .................................3,7,9
2 Connection for syringe...........................3
3 Feedthrough for aspirating tubing ......... 3
4 Aspirating tubing..............................3,7,9
5 Feedthrough for capillaries .................... 3
6 Connection for drain tube .....................3
7 Feedthrough for capillaries .................... 3
8 Connection to purge valve ....................3
9 Mains pilot lamp.....................................3
10 Bottle rack ...........................................3,5
11 Opening for detector cable....................5
12 Opening for inlet capillaries ...................5
13 Opening for outlet capillaries.................5
14 Connection for drain tube ......................5
15 Knurled screw ........................................5
16 Rear panel opening ...............................5
17 Detachable rear panel ...........................5
18 Transport security screws ...................... 5
19 Mains switch .....................................5,20
20 Mains connection plug .....................5,20
21 Fuse holder ....................................... 5,20
22 RS232 interface...................................... 5
23 Connection for detector block ...............5
24 Remote interface.................................... 5
25 Serial number.........................................5
26 Inlet capillary for injector ................7,9,26
27 Mounting rail .............................7,9,37,40
28 Column connection
capillary ...........................7,9,32,34,37,40
29 Sample loop........................................7,9
30 Connection capillary to syringe ..........7,9
31 Rotary nipple for aspirating tube ........7,9
32 Injection valve.......................7,9,26,37,40
33 PEEK coupling ............................... 7,9,40
34 Leak detector ......................................7,9
35 Connection capillary .....................7,9,26
36 Filter unit PEEK ....................7,9,18,26,40
37 Connection capillary ......................7,9,26
38 Connection capillary ...........................7,9
39 Purge valve.....................................7,9,26
40 Aspirating capillary..............................7,9
41 Fastening screws ................................7,9
42 Pump head...................................7,9,177
43 Connection capillary............................7,9
44 Connection capillary............................7,9
45 Inlet capillary for
detector block .......................... 7,9,37,40
46 Detector block .......................... 7,9,37,40
47 Suppressor module...........................9,40
48 Tubing cartridge ...........................9,39,41
49 Contact pressure lever .................9,39,41
50 Holding clamp...................................9,41
51 Snap-action lever .........................9,39,41
52 Pump drive ........................................9,41
53 Mounting pin .....................................9,41
54 Compression fitting .... 17,18,32,34,39,42
55 Compression fitting ..............................17
56 Capillary..................................... 17,18,34
57 Filter-Screw of Filter Unit .................18,39
58 Filter.................................................18,39
59 Filter-Housing of Filter Unit ..................18
60 Pulsation dampener .............................26
61 Connection to injection valve ...............26
62 Connection to purge valve ...................26
63 Aspirating tubing ..................................28
64 Tubing nipple........................................28
65 Threaded stopper.................................28
66 Bottle attachment .................................28
67 Eluent bottle..........................................28
68 Aspirating filter......................................28
69 CO
absorber .......................................28
2
70 Cotton wool ..........................................28
71 SGJ clip ................................................28
72 Absorber tube.......................................28
73 Manufit housing....................................32
74 Steel connector ....................................32
75 PTFE gasket .........................................32
76 2 Steel meshes.....................................32
77 Precolumn cartridge.............................32
78 Steel spacer .........................................32
761 Compact IC
VII
Table of contents
79 4 Steel meshes ....................................32
80 Manufit pressure screw ....................... 32
81 Separating column .................... 32,37,40
82 End fitting............................................. 34
83 Screw cap for precolumn .................... 34
84 Sleeve for precolumn cartridge ...........34
85 Precolumn cartridge ............................34
86 Connection piece................................. 34
87 Screw cap for column.......................... 34
88 Column holder ................................37,40
89 Aspirating tubing for H
90 Aspirating tubing for H
O........... 39,40,42
2
....... 39,40,42
2SO4
91 Coupling ......................................... 39,40
92 Pump tubing for H
93 Pump tubing for H
................... 39,40
2SO4
O ......................39,40
2
94 Stopper ................................................ 39
95 PTFE tubing ....................................39,40
96 Suppressor inlet capillary
for eluent ......................................... 41,43
97 Suppressor outlet capillary
for eluent ......................................... 41,43
98 Suppressor inlet capillary
for H
O ............................................41,43
2
99 Suppressor inlet capillary
for H
.................................... 39,41,43
2SO4
100 Suppressor outlet capillary
for H
O ............................................41,43
2
101 Suppressor outlet capillary
for H
......................................... 41,43
2SO4
102 Bottle attachment.................................42
103 Supply bottle ........................................42
104 Screw..................................................177
105 Zircon piston ......................................177
106 Spring retainer.................................... 177
107 Spring.................................................177
108 Piston cartridge..................................177
109 Piston guide sleeve............................177
110 Sapphire supporting ring ................... 177
111 Piston guide sleeve............................177
112 Piston seal.......................................... 177
113 Inlet valve ....................................177,179
114 Outlet valve..................................177,179
115 Screw holder ......................................177
116 Special tool ........................................ 177
117 Special tool ........................................ 177
118 Valve housing..................................... 179
119 Sealing ring ........................................179
120 Sleeve................................................. 179
121 Sapphire sleeve .................................179
122 Sapphire sphere.................................179
123 Ceramic holder...................................179
124 Seal ....................................................179
125 Screw nut ...........................................183
126 Connection piece...............................183
127 Suppressor rotor ................................ 183
128 Suppressor holder .............................183
761 Compact IC
VIII
1.1 Instrument description
1 Introduction
1.1 Instrument description
The 761 Compact IC is a PC-controlled system for ion chromatographic analyses. The two following versions are available:
• 2.761.0010 Compact IC without
• 2.761.0020 Compact IC with
The extremely compact housing of the 761 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 766 IC Sample Processor
• 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 25 MPa (250 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 761 Compact
IC can accommodate them all
suppressor module
suppressor module
761 Compact IC
• Suppressor – the Metrohm Suppressor Module (MSM) is already
integrated in the 2.761.0020 Compact IC – pressure-resistant, with
fully automatic regeneration, highest performance and optimal reproducibility
• Peristaltic pump – integrated two-channel peristaltic pump with a
flow rate of 0.5 … 0.6 mL/min for regeneration and rinsing of the
suppressor module built into the 2.761.0020 Compact IC
• 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.
All components which come into contact with eluent and sample are
metal-free.
1
1 Introduction
The operation of the 761 Compact IC takes place via a PC connected
to the RS232 interface with the help of the control and evaluation program «761 Compact IC». 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 such as the 750 Autosampler
or the 766 IC Sample Processor via the remote interface.
About 80 prepared system configurations for more than 300 applications are already permanently stored and additional new applications
can be downloaded at any time from the Internet under
«www.metrohm.ch».
The operating software for the 761 Compact IC 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 programm supplied can be used
to save and handle results and chromatograms produced by the «761
Compact IC» 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.
761 Compact IC
2
1.2 Parts and controls
1.2 Parts and controls
10
761 Compact IC
1
2
3
POWER
89 76 5
Fig. 1
: Front of the 761 Compact IC
1
Door to interior 6 Connection for drain tube
for discharge of spilled liquid from the
interior
2 Connection for 6.2816.020 Syringe
for aspiration of the sample
7 Feedthrough for capillaries
4
3 Feedthrough for aspirating tubing 8 Connection to purge valve
4 Aspirating tubing
for sample
5 Feedthrough for capillaries 10 Bottle rack
761 Compact IC
9 Mains pilot lamp
lit up when instrument switched on
for holding supply bottles with eluent,
regeneration solution, and rinsing
solution
3
1 Introduction
15
15
11
13 14 13 10
12 12 11
Waste B
Waste A
15
16
17
15
25
24
23a
23
Type 1.761.
WARNING - Fire Hazard -
For continued protection replace only
with the same type and rating of fuse
Analog Output
Remote
Detector Block
RS 232
Made by Metrohm Herisau Switzerland
22
100-120V:
220-240V:
Transport security scre ws
f = 50-60 Hz
S = 100 VA
Fuse
1,0A(T)
0,5A(T)
18
19
20
21
: Rear of the 761 Compact IC
Fig. 2
761 Compact IC
4
1.2 Parts and controls
10 Bottle rack
for holding supply bottles with eluent,
regeneration solution, and rinsing
18 Transport security screws
to secure the pump head when the
instrument is transported
solution
Opening for detector cable 19 Mains switch
11
to switch instrument on and off:
I = ON 0 = OFF
12 Opening for inlet capillaries
for supply of eluent, regeneration
20 Mains connection plug
mains connection, see section 2.4
solution, and rinsing solution into the
inner compartment
13 Opening for outlet capillaries
for discharge of eluent, regeneration
21 Fuse holder
changing the fuses, see section 2.4
solution, and rinsing solution from the
inner compartment
14 Connection for drain tube
for discharge of spilled liquid from the
22 RS232 interface
connection of the PC
bottle rack
15 Knurled screw
for fastening the rear panel 17
16 Rear panel opening
(closed with plastic stopper) for
additional supply and discharge lines to
and from the inner compartment
17 Detachable rear panel
access to upper part of inner
compartment
23
Connection for detector block
23a
Analog output for measuring
signal
24 Remote interface
remote I/O lines for connection of
external devices
25 Serial number
761 Compact IC
5
1 Introduction
46
45
44
43
42
41
40
39
38
1
26
27
28
29
30
31
4
27
32
36 35 34
37
: Interior of the 2.761.0010 Compact IC
Fig. 3
(with permanently attached accessories and
1.733.0110 Detector block)
761 Compact IC
6
33
1.2 Parts and controls
1 Door to interior 36 Filter unit PEEK (6.2821.120)
Aspirating tubing
4
for aspirating the sample;
6.1803.020 PTFE tubing,
length L = 52 cm
26 Inlet capillary for injector
6.1831.010 PEEK capillary,
length L = 24 cm
27 Mounting rail
for 6.2027.0X0 column holder
28 Column connection capillary
6.1831.010 PEEK capillary,
length L = 30 cm
29 Sample loop 10 µL
6.1825.230 PEEK sample loop
30 Connection capillary to syringe
6.1803.020 PTFE tubing,
length L = 30 cm
37 Connection capillary
6.1831.010 PEEK capillary,
length L = 13 cm
38 Connection capillary
6.1831.010 PEEK capillary,
length L = 15 cm
39 Purge valve
40 Aspirating capillary
Connection for 6.1834.010 aspirating
tubing
41 Fastening screws
for pump head 42
42 Pump head (6.2824.100)
31 Rotary nipple for aspirating tube
for fixing the aspirating tube
43 Connection capillary
Connection pump head – purge
valve, fixed mounting
32 Injection valve
33 PEEK coupling (6.2744.040)
44 Connection capillary
in pump head, fixed mounting
45 Inlet capillary for detector block
PEEK capillary, fixed mounting
34 Leak detector 46 Detector block (1.732.0110)
35 Connection capillary
6.1831.010 PEEK capillary,
length L = 13 cm
761 Compact IC
7
1 Introduction
46
45
44
43
42
41
40
39
38
1
26
27
28
29
47
30
31
4
27
32
48
36 35 34
37
: Interior of the 2.761.0020 Compact IC
Fig. 4
(with permanently attached accessories and
1.733.0110 Detector block)
761 Compact IC
8
33
53 52
5051
49
1.2 Parts and controls
1 Door to interior 39 Purge valve
Aspirating tubing
4
for aspirating the sample;
6.1803.020 PTFE tubing,
length L = 52 cm
26 Inlet capillary for injector
6.1831.010 PEEK capillary,
length L = 24 cm
27 Mounting rail
for 6.2027.0X0 column holder
28 Column connection capillary
6.1831.010 PEEK capillary,
length L = 30 cm
29 Sample loop 20 µL
6.1825.210 PEEK sample loop
30 Connection capillary to syringe
6.1803.020 PTFE tubing,
length L = 30 cm
40 Aspirating capillary
Connection for 6.1834.010 aspirating
tubing
41 Fastening screws
for pump head 42
42 Pump head (6.2824.100)
43 Connection capillary
Connection pump head – purge
valve, fixed mounting
44 Connection capillary
in pump head, fixed mounting
45 Inlet capillary for detector block
PEEK capillary, fixed mounting
31 Rotary nipple for aspirating tube
46 Detector block (1.732.0110)
for fixing the aspirating tube
32 Injection valve
47 Suppressor module
(inlet and outlet capillaries are not
shown)
33 PEEK coupling (6.2744.040)
48 Tubing cartridge (6.2755.000)
for 6.1826.060 pump tubing
34 Leak detector 49 Contact pressure lever
for adjusting the contact pressure
35 Connection capillary
6.1831.010 PEEK capillary,
length L = 13 cm
50 Holding clamp
for locking the tubing cartridge into
place
36 Filter unit PEEK (6.2821.120) 51 Snap-action lever
for releasing the tubing cartridge
37 Connection capillary
6.1831.010 PEEK capillary,
52 Pump drive
roller head with contact rollers
length L = 13 cm
38 Connection capillary
6.1831.030 PEEK capillary,
length L = 20 cm
761 Compact IC
53 Mounting pin
for attaching the tubing cartridges
9
1 Introduction
1.3 Information on the Instructions for Use
Please read through these Instructions for Use carefully before you put
the 761 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 8.761.1063 Instructions for Use for the 761 Compact IC pro-
vide a comprehensive overview of the installation, startup procedure,
operation, fault rectification and technical specifications of this instrument. The Instructions for Use are organized as follows:
Section 1 Introduction
General description of instrument, parts and controls
and safety notes
Section 2 Installation
Installation of instrument, accessories,
and external devices
Section 3 Operating tutorial
Introduction to the operation using an example
Section 4 Operation
Detailed description of the operation
Section 5 Notes – Maintenance – Faults
Notes on ion chromatography, maintenance, fault rectification, diagnostic tests, validation
Section 6 Appendix
Technical data, standard equipment, options, warranty,
declarations of conformity, index
To find the required information on the instruments, you will find it an
advantage to use either the Table of contents or the Index at the
back.
As a supplement to the Instructions for Use, the Metrohm Monograph
8.732.2003 "Ion chromatography" is also supplied. This provides an
introduction to the theoretical fundamentals and general information on
separating columns and sample pretreatment.
The 8.732.2013 IC Applications Collection is also supplied; this contains all the Application Notes on the subject of ion chromatography.
Each of these applications can be carried out directly with the 761
Compact IC by loading the system file with the same name. The Applications Collection can be updated at any time by downloading the latest applications from the Internet under «www.metrohm.ch».
You will find detailed information on the separating columns available
from Metrohm and on special IC applications in the relevant "Applica-
tion Bulletins", which are available on request free of charge from your
Metrohm agency.
761 Compact IC
10
1.3 Information on the Instructions for Use
1.3.2 Notation and pictograms
The following notations and pictograms (symbols) are used in these Instructions for Use:
Range Menu item, parameter or entry
value
SYSTEM STATE Program window
<OK> Button
[ Ctrl ] Key
35 Part or control of 761
12 Part or control of 750
26 Part or control of 766
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.
761 Compact IC
Comment
This symbol marks additional
information and tips.
11
1 Introduction
1.4 Safety notes
1.4.1 Electrical safety
While electrical safety in the handling of the 761 Compact IC is assured
in the context of the specifications IEC 1010-1 (protection class 1, degree of protection IP20), the following points should be 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 761 Compact IC
If the 761 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. Hence, always disconnect the instrument from all voltage
sources before you open it and ensure that the mains cable is
disconnected from mains connection 20 !
• 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 761 Compact IC, you should earth yourself and any tools
you are using by touching an earthed 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.
761 Compact IC
12
2.1 Overview
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 sect. 2.3
Mains connection sect. 2.4
Connecting PC sect. 2.5
Connecting high pr. pump sect 2.6
Precolumn
No
Installing sample loop sect. 2.7.6
Connecting column sect. 2.7.7/8
Suppressor Connecting suppressor module sect. 2.8
No
Conditioning sect. 2.9
Connecting external devices sect. 2.10
Yes
Yes
Precolumn with cartridge head sect. 2.7.2
Precolumn with cartridge holder sect. 2.7.3
IC anion precolumn SUPERSEP sect. 2.7.4
2.1.2 Connections in the 761 Compact IC
The two following illustrations show the internal connections in the 761
Compact IC in schematic form. The meanings of the various numbered
components are given in the detailed illustrations and descriptions in
sections 2.2 – 2.10.
761 Compact IC
13
2 Installation
28 81 45 46
63
40
39
42
37
Eluent
44 43
38
66
67
68
36 35
60
26 29 32
30
Column
Injection valve
4
Sample
Detector
Waste
: Connecting diagram for 2.761.0010 Compact IC without suppressor
Fig. 5
44 43
28 81 96
26 29 32
97 33 45 46
42
Detector
98
100
40
36 35
Column
47
101
99
37
89
36
9191 93 95
63
39
66
38
60
30
90
102
103
92
4
67
102
68
H
OH2SO
Eluent
: Connecting diagram for 2.761.0020 Compact IC with suppressor
Fig. 6
761 Compact IC
14
Sample
4
2
103
Waste
2.2 Setting up the instrument
2.2 Setting up the instrument
2.2.1 Packaging
The 761 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 6.2). In the case of transport damage, see
instructions in section 6.4.1 "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.
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 761 Compact IC; it must be inserted in the instrument and
connected up. Proceed as follows:
1 Note the cell constant
• The cell constant c = XX,X /cm is printed on the rear of the
detector block. Note this value; it must subsequently be entered in the software in order to ensure that an exact display
of the conductivity is obtained (see section 2.5.3).
761 Compact IC
2 Install detector block
• Unscrew the four knurled screws 15 from the top rear panel
17 of the 761 Compact IC and remove rear panel (see Fig. 2).
• Position detector block 46 from the back in the space pro-
vided in the 761 Compact IC and push fully to the front (see
Fig. 3 and Fig. 4).
15
2 Installation
• Insert the cable permanently attached to the detector block
46 in one of the openings 11 and the outlet capillary in one of
the openings 13 of the rear panel 17.
• Replace rear panel 17 and screw to the 761 Compact IC
using the four knurled screws 15.
3 Connect detector block
• Plug the gray connecting cable permanently attached to the
detector block 46 into connection 23 "Detector Block" of the
761 Compact IC and fasten to the instrument by tightening
the screws in the cable connector (see Fig. 2).
4 Connect waste container
• Lead the outlet capillary of the detector block 46 to a suffi-
ciently large waste container and fix in place.
2.3.2 Connection of syringe and aspirating tubing
For manual filling of the sample loop 29 mounted on the injection valve,
the 6.2816.020 Syringe and the PTFE aspirating tubing 4 already
screwed to the valve are needed. These accessories are mounted or
adjusted as follows:
1 Connect syringe
• Push 6.2816.020 Syringe (without needle) as far as it will go
into connection socket 2 (see Fig. 1).
2 Adjust aspirating tubing
• Loosen the rotary nipple 31 screwed onto the interior side of
feedthrough 3 (see Fig. 3 and Fig. 4).
• Pull PTFE aspirating tubing 4 (see Fig. 3 and Fig. 4) by hand
out of feedthrough 3 as far as desired.
• Retighten rotary nipple 31 on the interior side of feedthrough
3 to fix the aspirating tubing 4 in place.
2.3.3 Connection of the drain tube for the inner compartment
The 761 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 6
(see Fig. 1).
2 Lead drain tube to collecting vessel
• Lead the other end of the drain tube to a suitable collecting
vessel and fix in place.
761 Compact IC
16
2.3 Attaching the accessories
2.3.4 Connection of the drain tube for bottle rack
The 761 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 14
(see Fig. 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
1
6.1831.010 PEEK capillaries (i.d. = 0.25 mm, e.d. =
which are connected using either 6.2744.010 PEEK compression fit-
tings (long) or 6.2744.070 PEEK compression fittings (short).
These PEEK connectors can also be used to connect 6.1822.010 PTFE
microcapillaries (i.d. = 0.3 mm). Proceed as follows:
/16") are used
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 Fig. 7.
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 Compression fitting (6.2744.010)
55 Compression fitting (6.2744.070)
54 56 55
Fig. 7
: Connectors for capillaries
761 Compact IC
56 Capillary
6.1831.010 PEEK capillary or
6.1822.010 PTFE microcapillary
17
2 Installation
2.3.6 Filter unit PEEK
One 6.2821.120 Filter unit PEEK (see Fig. 8) is already installed be-
tween the high-pressure pump and the injection valve at the 761 Compact IC. This filter unit serves to avoid contamination by abrasive particles of the piston seals.
The two other filter units PEEK supplied with the 2.761.0020 Compact
IC (with suppressor) are installed between the pump tubings of the
peristaltic pump and the inlet capillaries for regeneration and rinsing solution (see section 2.8.2). These filter units serve to protect the suppressor module from foreign particles and bacterial growth.
The Filter unit PEEK 36 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 (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).
For the connection of the filter unit, please note the flow direction
arrow printed on the housing.
36
56 54
36 Filter unit PEEK (6.2821.120) 57 Filter-Screw of Filter Unit
54 Compression fitting (6.2744.010) 58 Filter 6.2821.130
56 Capillary
6.1831.010 PEEK capillary or
6.1822.010 PTFE microcapillary
57
Fig. 8
: 6.2821.120 Filter unit PEEK
58
Part of 6.2821.120 Filter unit
Part of 6.2821.120 Filter unit
59 Filter-Housing of Filter Unit
Part of 6.2821.120 Filter unit
59 54 56
761 Compact IC
18
2.4 Mains connection
2.4 Mains connection
Follow the instructions below for connecting to the power supply. If
the instrument is operated with a mains voltage set wrongly and/or
wrong mains fuse, there is a danger of fire!
2.4.1 Setting the mains voltage
Before switching on the 761 Compact IC for the first time, check that
the mains voltage set on the instrument (see Fig. 9) matches the local
mains voltage. If this is not
on the instrument as follows:
1 Disconnect mains cable
Disconnect mains cable from mains connection plug 20 of the
761 Compact IC.
the case, you must reset the mains voltage
2 Remove fuse holder
Using a screwdriver, loosen fuse holder 21 below the mains
connection plug 20 and take out completely.
3 Check and change fuse if necessary
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 1.0 A (slow-blow) Metrohm No. U.600.0016
220…240 V 0.5 A (slow-blow) Metrohm No. U.600.0013
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 761 Compact IC so that the corresponding mains voltage
range can be read normally and the adjacent white arrow points
to the white bar imprinted below the fuse holder (see Fig. 9).
761 Compact IC
19
2 Installation
100 – 120 V 220 – 240 V
2.4.2 Fuses
19
19 Mains switch
20
21
220 - 240 V
Fig. 9
: Setting the mains voltage
100 - 120 V
100 - 120 V
One of the two fuses 1 A/slow-blow for 100…120 V or 0.5 A/slow-blow
for 220…240 V is installed in fuse holder 21 of the 761 Compact IC 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, process as described in section 2.4.1.
220 - 240 V
20 Mains connec-
tion plug
21 Fuse holder
2.4.3 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 20 of the 761 Compact IC (see Fig. 9).
2.4.4 On/off switching of the instrument
The 761 Compact IC is switched on and off using mains switch 19.
When the instrument is switched on, the mains pilot lamp 9 lights up.
761 Compact IC
20
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