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 [e-mail]

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	10
		1.3.2	11
	1.4	Safety notes...........................................................................................................	12
		1.4.1	12
		1.4.2	12
2	Installation ..........................................................................................................		13
	2.1	Overview	13
		2.1.1	13
		2.1.2 Connections in the 761 Compact IC ....................................................	13
	2.2	Setting up ....................................................................................the instrument	15
		2.2.1 .............................................................................................	15
		2.2.2 ....................................................................................................	15
		2.2.3 ................................................................................................	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 .....................................................................................	18
	2.4	Mains connection .................................................................................................	19
		2.4.1 .....................................................................Setting the mains voltage	19
		2.4.2 ....................................................................................................	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 .................................................................................	21
		2.5.2 ..............................................................................	21
		2.5.3 .......................................................................................	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
	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

761 Compact IC

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

II

761 Compact IC

			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

IV

761 Compact IC

			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
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

761 Compact IC

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
Fig. 9:	Setting the mains voltage .............................................................................	20
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
Fig. 18:	Connections at suppressor module .............................................................	43
Fig. 19:	Components of the pump head .................................................................	177
Fig. 20:	Replacement of the piston seal 112 ..........................................................	177
Fig. 21:	Components of inlet valve 113 and outlet valve 114.................................	179
Fig. 22:	Assembling the suppressor........................................................................	183

VI

761 Compact IC

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	CO2 absorber .......................................	28
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 H2O...........	39,40,42
90	Aspirating tubing for H2SO4 .......	39,40,42
91	Coupling .........................................	39,40
92	Pump tubing for H2SO4 ...................	39,40
93	Pump tubing for H2O ......................	39,40
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 H2O ............................................	41,43
99	Suppressor inlet capillary
	for H2SO4....................................	39,41,43
100	Suppressor outlet capillary
	for H2O ............................................	41,43
101	Suppressor outlet capillary
	for H2SO4.........................................	41,43

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

VIII

761 Compact IC

1.1 Instrument description

1 Introduction

1.1Instrument 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 suppressor module

•2.761.0020 Compact IC with suppressor module

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 – 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.

761 Compact IC

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.

2	761 Compact IC

1.2 Parts and controls

1.2Parts and controls

10

761 Compact IC

1

2

3

4

POWER

	9				8	7	6	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					7	Feedthrough for capillaries
	for aspiration of the sample
3	Feedthrough for aspirating tubing					8	Connection to purge valve
4	Aspirating tubing					9	Mains pilot lamp
	for sample						lit up when instrument switched on
5	Feedthrough for capillaries					10	Bottle rack
							for holding supply bottles with eluent,
							regeneration solution, and rinsing
							solution

761 Compact IC

3

1 Introduction

11	12	13	14	13	12	10	11

15	15
Waste B	Waste A

16

15 25

Transport security screws

	Type 1.761.
	WARNING - Fire Hazard -
24	For continued protection replaceonly
	with the same type and rating of fuse
23a			f = 50-60 Hz
	Analog Output		S = 100 VA
		Remote	Fuse
		100-120V:	1,0A(T)
23		220-240V:	0,5A(T)
	Detector Block	RS 232

Made by Metrohm Herisau Switzerland

17

15

18

19

20

21

22

Fig. 2: Rear of the 761 Compact IC

4	761 Compact IC

1.2 Parts and controls

10Bottle rack

for holding supply bottles with eluent, regeneration solution, and rinsing solution

18Transport security screws

to secure the pump head when the instrument is transported

11	Opening for detector cable	19	Mains switch
			to switch instrument on and off:
			I = ON 0 = OFF
12	Opening for inlet capillaries	20	Mains connection plug
	for supply of eluent, regeneration		mains connection, see section 2.4
	solution, and rinsing solution into the
	inner compartment
13	Opening for outlet capillaries	21	Fuse holder
	for discharge of eluent, regeneration		changing the fuses, see section 2.4
	solution, and rinsing solution from the
	inner compartment
14	Connection for drain tube	22	RS232 interface
	for discharge of spilled liquid from the		connection of the PC
	bottle rack
15	Knurled screw	23	Connection for detector block
	for fastening the rear panel 17
		23a	Analog output for measuring
			signal
16	Rear panel opening	24	Remote interface
	(closed with plastic stopper) for		remote I/O lines for connection of
	additional supply and discharge lines to		external devices
	and from the inner compartment
17	Detachable rear panel	25	Serial number
	access to upper part of inner
	compartment

761 Compact IC

5

1 Introduction

46
45	1
44	26
43	27
	28
42	29

41
	30
	31
40	4
39	27
	32
38

37		36	35	34	33

Fig. 3: Interior of the 2.761.0010 Compact IC

(with permanently attached accessories and 1.733.0110 Detector block)

6	761 Compact IC

				1.2 Parts and controls
1		Door to interior	36	Filter unit PEEK (6.2821.120)
4		Aspirating tubing	37	Connection capillary
		for aspirating the sample;		6.1831.010 PEEK capillary,
		6.1803.020 PTFE tubing,		length L = 13 cm
		length L = 52 cm
26		Inlet capillary for injector	38	Connection capillary
		6.1831.010 PEEK capillary,		6.1831.010 PEEK capillary,
		length L = 24 cm		length L = 15 cm
27		Mounting rail	39	Purge valve
		for 6.2027.0X0 column holder
28		Column connection capillary	40	Aspirating capillary
		6.1831.010 PEEK capillary,		Connection for 6.1834.010 aspirating
		length L = 30 cm		tubing
29		Sample loop 10 L	41	Fastening screws
		6.1825.230 PEEK sample loop		for pump head 42
30		Connection capillary to syringe	42	Pump head (6.2824.100)
		6.1803.020 PTFE tubing,
		length L = 30 cm
31		Rotary nipple for aspirating tube	43	Connection capillary
		for fixing the aspirating tube		Connection pump head – purge
				valve, fixed mounting
32		Injection valve	44	Connection capillary
				in pump head, fixed mounting
33		PEEK coupling (6.2744.040)	45	Inlet capillary for detector block
				PEEK capillary, fixed mounting
34		Leak detector	46	Detector block (1.732.0110)

35Connection 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

49

37	36 35	34 33	53	52	51		50

Fig. 4: Interior of the 2.761.0020 Compact IC

(with permanently attached accessories and 1.733.0110 Detector block)

8	761 Compact IC

				1.2 Parts and controls
1		Door to interior	39	Purge valve
4		Aspirating tubing	40	Aspirating capillary
		for aspirating the sample;		Connection for 6.1834.010 aspirating
		6.1803.020 PTFE tubing,		tubing
		length L = 52 cm
26		Inlet capillary for injector	41	Fastening screws
		6.1831.010 PEEK capillary,		for pump head 42
		length L = 24 cm
27		Mounting rail	42	Pump head (6.2824.100)
		for 6.2027.0X0 column holder
28		Column connection capillary	43	Connection capillary
		6.1831.010 PEEK capillary,		Connection pump head – purge
		length L = 30 cm		valve, fixed mounting
29		Sample loop 20 L	44	Connection capillary
		6.1825.210 PEEK sample loop		in pump head, fixed mounting
30		Connection capillary to syringe	45	Inlet capillary for detector block
		6.1803.020 PTFE tubing,		PEEK capillary, fixed mounting
		length L = 30 cm
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	50	Holding clamp
		6.1831.010 PEEK capillary,		for locking the tubing cartridge into
		length L = 13 cm		place
36		Filter unit PEEK (6.2821.120)	51	Snap-action lever
				for releasing the tubing cartridge
37		Connection capillary	52	Pump drive
		6.1831.010 PEEK capillary,		roller head with contact rollers
		length L = 13 cm
38		Connection capillary	53	Mounting pin
		6.1831.030 PEEK capillary,		for attaching the tubing cartridges
		length L = 20 cm

761 Compact IC

9

1 Introduction

1.3Information 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.

1.3.1Organization

These 8.761.1063 Instructions for Use for the 761 Compact IC provide 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 "Application Bulletins", which are available on request free of charge from your Metrohm agency.

10	761 Compact IC

1.3 Information on the Instructions for Use

1.3.2Notation 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 correct-
					ly.
					Caution
					This symbol marks important
					information. First read the associ-
					ated directions before you conti-
					nue.
					Comment
					This symbol marks additional
					information and tips.

761 Compact IC

11

1 Introduction

1.4Safety notes

1.4.1Electrical 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 instructions 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.

1.4.2General 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.

12	761 Compact IC

2.1 Overview

2 Installation

2.1Overview

2.1.1Flow 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			Yes
	No
Installing sample loop			sect. 2.7.6
Connecting column			sect. 2.7.7/8
Suppressor			Yes
	No
Conditioning			sect. 2.9

Connecting external devices sect. 2.10

Precolumn with cartridge head	sect. 2.7.2
Precolumn with cartridge holder	sect. 2.7.3
IC anion precolumn SUPERSEP	sect. 2.7.4

Connecting suppressor module	sect. 2.8

2.1.2Connections 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

44

43

26

29

32

42

Column Detector

40

36	35	Injection valve

37

39

63												38																			4
																60		30
												66
												67
												68
												Eluent																				Sample														Waste
		Fig. 5: Connecting diagram for 2.761.0010 Compact IC without suppressor
																								28							81					96				97 33						45			46
44												43				26		29						32
42																																																	Detector
40																															Column
														36		35															101									47						98			100
																								99
37																																				36
39																								4							92
63
												38												90
														60		30
						66																		102							91					89				93 91						95
																								103
												67																												102
												68																												103									Waste
																	Sample														H2SO4					H2O
									Eluent

Fig. 6: Connecting diagram for 2.761.0020 Compact IC with suppressor

14	761 Compact IC

2.2 Setting up the instrument

2.2Setting up the instrument

2.2.1Packaging

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.

2.2.2Check

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".

2.2.3Location

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.

2.3Attaching the accessories

2.3.1Connection 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:

1Note 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).

2Install 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 provided in the 761 Compact IC and push fully to the front (see

Fig. 3 and Fig. 4).

761 Compact IC

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.

3Connect 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).

4Connect waste container

•Lead the outlet capillary of the detector block 46 to a sufficiently large waste container and fix in place.

2.3.2Connection 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:

1Connect syringe

•Push 6.2816.020 Syringe (without needle) as far as it will go into connection socket 2 (see Fig. 1).

2Adjust 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.

2.3.3Connection 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:

1Connect drain tube

•Mount 6.1816.020 Silicone tubing on connection nipple 6 (see Fig. 1).

2Lead drain tube to collecting vessel

•Lead the other end of the drain tube to a suitable collecting vessel and fix in place.

16	761 Compact IC

2.3 Attaching the accessories

2.3.4Connection 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:

1Connect drain tube

•Mount 6.1816.020 Silicone tubing on connection nipple 14 (see Fig. 2).

2Lead drain tube to collecting vessel

•Lead the other end of the drain tube to a suitable collecting vessel and fix in place.

2.3.5Connection of PEEK capillaries

For the connections between high-pressure pump and detector block 6.1831.010 PEEK capillaries (i.d. = 0.25 mm, e.d. = 1/16") are used which are connected using either 6.2744.010 PEEK compression fittings (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:

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.

1Mount 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.

2Insert capillary in connection

Push capillary end in the corresponding connection as far as it will go (to avoid dead volume).

3Tighten 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)
						56					Capillary
54		56				55					6.1831.010 PEEK capillary or

6.1822.010 PTFE microcapillary

Fig. 7: Connectors for capillaries

761 Compact IC

17

2 Installation

2.3.6Filter unit PEEK

One 6.2821.120 Filter unit PEEK (see Fig. 8) is already installed between 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		57						58				59		54				56

Fig. 8: 6.2821.120 Filter unit PEEK

36	Filter unit PEEK (6.2821.120)	57	Filter-Screw of Filter Unit
			Part of 6.2821.120 Filter unit
54	Compression fitting (6.2744.010)	58	Filter 6.2821.130
			Part of 6.2821.120 Filter unit
56	Capillary	59	Filter-Housing of Filter Unit
	6.1831.010 PEEK capillary or		Part of 6.2821.120 Filter unit
	6.1822.010 PTFE microcapillary

18	761 Compact IC

2.4 Mains connection

2.4Mains 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!

2.4.1Setting 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 the case, you must reset the mains voltage on the instrument as follows:

1Disconnect mains cable

Disconnect mains cable from mains connection plug 20 of the 761 Compact IC.

2Remove fuse holder

Using a screwdriver, loosen fuse holder 21 below the mains connection plug 20 and take out completely.

3Check 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

4Insert fuse

Change fuse if necessary and reinsert in fuse holder 21.

5Install 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

220 – 240 V

100 – 120 V

19

20

21

100-120V

220-240V

220 - 240 V

100 - 120 V

Fig. 9: Setting the mains voltage

2.4.2Fuses

19Mains switch

20Mains connection plug

21Fuse holder

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.

2.4.3Mains 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).

2.4.4On/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.

20	761 Compact IC