Metrohm 792 Basic IC Manual de usuario

CH-9101 Herisau/Switzerland

Phone ++41 71 353 85 85

Fax ++41 71 353 89 01

Internet www.metrohm.com

E-Mail [email protected]

792 Basic IC

Program «792 PC Software 1.0»

POWER

Basic IC792

Basic

BasicBasic

Basic

8.792.1003 Instructions for Use

11.04.2001 / dö

Table of contents

792 Basic IC

Table of contents

1Introduction............................................................................................................1

1.1 Instrument description.......................................................................................... 1

1.2 Parts and controls.................................................................................................. 3

1.3 Information on the Instructions for Use............................................................. 8

1.3.1 Organization ........................................................................................... 8

1.3.2 Notation and pictograms........................................................................ 9

1.4 Safety notes .......................................................................................................... 10

1.4.1 Electrical safety..................................................................................... 10

1.4.2 General precautionary rules ................................................................. 10

2Installation .......................................................................................................... 11

2.1 Overview ................................................................................................................ 11

2.1.1 Flow chart ............................................................................................. 11

2.1.2 Connections in the 792 Basic IC .......................................................... 11

2.2 Setting up the instrument ................................................................................... 13

2.2.1 Packaging............................................................................................. 13

2.2.2 Check.................................................................................................... 13

2.2.3 Location ................................................................................................ 13

2.3 Attaching the accessories .................................................................................. 13

2.3.1 Connection of detector block ............................................................... 13

2.3.2 Connection of syringe and aspirating tubing....................................... 14

2.3.3 Connection of the 6.5324.000 Bottle rack (option) .............................. 14

2.3.4 Connection of PEEK capillaries............................................................ 15

2.3.5 Filter unit PEEK ..................................................................................... 16

2.4 Mains connection ................................................................................................. 17

2.4.1 Setting the mains voltage ..................................................................... 17

2.4.2 Fuses .................................................................................................... 18

2.4.3 Mains cable and mains connection ..................................................... 18

2.4.4 On/off switching of the instrument ....................................................... 18

2.5 Connection to the PC .......................................................................................... 19

2.5.1 Connecting cable ................................................................................. 19

2.5.2 Software installation.............................................................................. 19

2.5.3 Basic settings ....................................................................................... 20

2.6 High-pressure pump............................................................................................ 23

2.6.1 Removing the transport security screws .............................................. 23

2.6.2 Installing the pulsation dampener (option) .......................................... 23

2.6.3 Connecting the eluent bottle ................................................................ 25

2.6.4 Deaerating the pump and rinsing the pulsation dampener................. 25

2.7 Precolumns and separating columns............................................................... 28

2.7.1 General information on precolumns..................................................... 28

2.7.2 Precolumns with twin cartridge holder ................................................. 28

2.7.3 Precolumn glass cartridges with cartridge holder ............................... 30

2.7.4 IC anion precolumn SUPERSEP .......................................................... 31

2.7.5 General information on separating columns........................................ 32

2.7.6 Selection of the sample loop................................................................ 32

2.7.7 Installation of the separating column without suppressor ................... 32

2.7.8 Installation of the separating column with suppressor ........................ 34

Table of contents

792 Basic IC

2.8 Suppressor module ............................................................................................. 35

2.8.1 General information on suppressor module........................................ 35

2.8.2 Preparation of the peristaltic pump...................................................... 35

2.8.3 Connection of supply bottles ............................................................... 38

2.8.4 Connection of the suppressor module ................................................ 39

2.9 Putting into operation ......................................................................................... 41

2.9.1 Putting into operation without suppressor ........................................... 41

2.9.2 Putting into operation with suppressor ................................................ 42

3Operating tutorial ....................................................................................... 45

3.1 Requirements ....................................................................................................... 45

3.2 Preparations.......................................................................................................... 46

3.3 Calibration ............................................................................................................. 47

3.4 Sample determination ......................................................................................... 54

4Operation............................................................................................................... 57

4.1 Fundamentals of the operation ......................................................................... 57

4.1.1 Starting/closing the program ............................................................... 57

4.1.2 Glossary................................................................................................ 58

4.1.3 Overview of program windows............................................................. 59

4.1.4 Main window elements......................................................................... 60

4.1.5 Icons of the main window..................................................................... 60

4.1.6 Overview of file types............................................................................ 61

4.1.7 Context sensitive menus ...................................................................... 62

4.1.8 Keyboard and mouse functions........................................................... 62

4.1.9 Help ...................................................................................................... 63

4.2 Instrument and software settings ..................................................................... 64

4.2.1 Fonts..................................................................................................... 64

4.2.2 Security system .................................................................................... 64

4.2.3 Global settings ..................................................................................... 65

4.2.4 COM port .............................................................................................. 67

4.3 Systems ................................................................................................................. 68

4.3.1 System window .................................................................................... 68

4.3.2 System file handling ............................................................................. 68

4.3.3 System functions .................................................................................. 69

Start/stop hardware and record baseline .................................... 69

Start/stop determinations............................................................. 69

Print system parameters .............................................................. 70

4.3.4 PC icon ................................................................................................. 71

4.3.5 Watch window ...................................................................................... 71

4.3.6 Instrument icon..................................................................................... 72

Menu options for instrument icon ................................................ 72

System parameters for disconnected system ............................. 72

Instrument control for connected system .................................... 73

Time program ............................................................................... 74

Configuration ................................................................................ 76

Hardware settings ........................................................................ 76

4.3.7 System state window............................................................................ 78

Status messages.......................................................................... 78

Error messages ............................................................................ 79

Table of contents

792 Basic IC

III

4.4 Methods ................................................................................................................. 80

4.4.1 Method file handling ............................................................................. 80

4.4.2 Passport................................................................................................ 80

General ......................................................................................... 81

Sample.......................................................................................... 82

Column ......................................................................................... 83

Eluent ............................................................................................ 84

Comment ...................................................................................... 84

Method Log .................................................................................. 85

Data Log ....................................................................................... 86

4.4.3 Method setup........................................................................................ 87

General ......................................................................................... 87

Processing.................................................................................... 87

Math .............................................................................................. 88

4.4.4 Integration............................................................................................. 90

Setup............................................................................................. 91

Events ........................................................................................... 92

4.4.5 Calibration and quantification............................................................... 94

General information ...................................................................... 94

Notations....................................................................................... 95

External standard calibration........................................................ 96

Component table.......................................................................... 96

Peak identification ........................................................................ 98

Concentration table .................................................................... 100

Calibration curve......................................................................... 102

Update calibration ...................................................................... 104

Load and save calibration data.................................................. 105

Import and export calibration data ............................................. 105

Put out calibration curves ........................................................... 105

4.4.6 Report output...................................................................................... 106

Report options ............................................................................ 106

4.5 Chromatograms..................................................................................................118

4.5.1 Chromatogram window ...................................................................... 118

4.5.2 Chromatogram file handling............................................................... 119

Open chromatogram .................................................................. 119

Save chromatogram................................................................... 120

Close chromatogram.................................................................. 120

Delete chromatogram................................................................. 120

Export chromatogram................................................................. 121

4.5.3 Graphical representation .................................................................... 122

Appearance ................................................................................ 122

Other graphical functions ........................................................... 126

4.5.4 Peak editor.......................................................................................... 127

Switching on/off the peak editor................................................. 127

Peak editor functions.................................................................. 127

Moving the cursor....................................................................... 128

4.5.5 Printing................................................................................................ 129

Page layout for printing .............................................................. 129

Printer settings ............................................................................ 130

Print preview ............................................................................... 130

Printing........................................................................................ 130

4.5.6 Miscellaneous functions ..................................................................... 130

Reintegration............................................................................... 130

Recalibration............................................................................... 130

Subtraction of a chromatogram ................................................. 131

Data compression ...................................................................... 131

Invert chromatogram .................................................................. 131

Table of contents

792 Basic IC

4.6 Batch reprocessing ........................................................................................... 132

4.6.1 Batch reprocessing queue file handling ............................................ 132

Open batch reprocessing queue ............................................... 132

Create new batch reprocessing queue...................................... 132

Save batch reprocessing queue ................................................ 132

4.6.2 Perform batch reprocessing............................................................... 133

Reprocess options window........................................................ 133

Merge chromatograms .............................................................. 136

4.6.3 Batch reprocessing queue editor....................................................... 137

Open batch reprocessing queue editor window ....................... 137

Batch reprocessing queue editor functions............................... 138

Print batch reprocessing queue................................................. 138

Close batch reprocessing queue editor .................................... 138

5Notes – Maintenance – Faults ................................................... 139

5.1 Practical notes on ion chromatography ........................................................ 139

5.1.1 Separating columns ........................................................................... 139

5.1.2 High-pressure pump .......................................................................... 140

5.1.3 Eluents ................................................................................................ 141

5.1.4 Peristaltic pump.................................................................................. 141

5.1.5 Suppressor module............................................................................ 142

5.1.6 Connections ....................................................................................... 142

5.2 Maintenance and servicing .............................................................................. 143

5.2.1 General information............................................................................ 143

5.2.2 Passivation ......................................................................................... 143

5.2.3 Recycling ............................................................................................ 144

5.2.4 Shutdown............................................................................................ 144

5.2.5 Changing separating columns........................................................... 144

5.2.6 Maintenance work at the pump head ................................................ 146

5.2.7 Regeneration of the suppressor module ........................................... 150

5.2.8 Cleaning the suppressor.................................................................... 151

5.2.9 Replacing the suppressor .................................................................. 153

5.2.10 Exchanging the pump tubing............................................................. 155

5.3 Faults and malfunctions ................................................................................... 156

5.3.1 Error messages .................................................................................. 156

5.3.2 Malfunctions and their rectification .................................................... 156

5.4 Diagnostic tests / Validation / GLP ................................................................. 158

Table of contents

792 Basic IC

6Appendix..............................................................................................................159

6.1 Technical data..................................................................................................... 159

6.1.1 Conductivity measurement................................................................. 159

6.1.2 Conductivity detector.......................................................................... 159

6.1.3 Injection valve ..................................................................................... 160

6.1.4 High-pressure pump .......................................................................... 160

6.1.5 Peristaltic pump .................................................................................. 161

6.1.6 Suppressor module ............................................................................ 161

6.1.7 RS232 interface .................................................................................. 161

6.1.8 Mains connection ............................................................................... 162

6.1.9 Safety specifications........................................................................... 162

6.1.10 Electromagnetic compatibility (EMC)................................................. 162

6.1.11 Ambient temperature.......................................................................... 163

6.1.12 Housing............................................................................................... 163

6.2 Standard equipment .......................................................................................... 164

6.3 Optional accessories.........................................................................................167

6.3.1 Accessories for 792 Basic IC ............................................................. 167

6.3.2 Separating columns and precolumns................................................ 169

6.3.3 Additional devices and cables ........................................................... 175

6.4 Warranty and conformity ..................................................................................176

6.4.1 Warranty.............................................................................................. 176

6.4.2 EU Declaration of conformity.............................................................. 177

6.4.3 Certificate of conformity and system validation ................................. 178

6.4 Index .....................................................................................................................179

Table of contents

792 Basic IC

List of figures

Fig. 1: Front of the 792 Basic IC ................................................................................ 3

Fig. 2: Rear of the 792 Basic IC................................................................................. 4

Fig. 3: Interior of the 792 Basic IC ............................................................................. 6

Fig. 4: Connecting diagram for 792 Basic IC without suppressor.......................... 12

Fig. 5: Connecting diagram for 792 Basic IC with suppressor ............................... 12

Fig. 6: Connectors for capillaries............................................................................. 15

Fig. 7: 6.2821.100 Filter unit PEEK .......................................................................... 16

Fig. 8: Setting the mains voltage ............................................................................. 18

Fig. 9: Connection of the pulsation dampener (option) .......................................... 24

Fig. 10: Installing precolumn cartridges .................................................................... 29

Fig. 11: Installation of precolumn glass cartridges with cartridge holder ................. 31

Fig. 12: Installation of column without suppressor.................................................... 33

Fig. 13: Installing pump tubings ................................................................................ 36

Fig. 14: Installation of column with suppressor......................................................... 37

Fig. 15: Connections at suppressor module ............................................................. 40

Fig. 16: Components of the pump head ................................................................. 147

Fig. 17: Replacement of the piston seal 89

8989

89............................................................. 147

Fig. 18: Components of inlet valve 90

9090

90 and outlet valve 91

9191

91 ..................................... 149

Fig. 19: Assembling the suppressor....................................................................... 153

Table of contents

792 Basic IC

VII

List of numbered parts and controls

1Door to interior ....................................3,6

2Mains pilot lamp.....................................3

3Feedthrough for syringe tubing .............3

4Feedthrough for aspirating tubing.........3

5Opening for detector cable....................4

6Rear panel opening ...............................4

7Opening for outlet capillaries.................4

8Knurled screw ........................................4

9Detachable rear panel ...........................4

1010

10 Transport security screws...................... 4

1111

11 Mains switch .....................................4,18

1212

12 Mains connection plug .....................4,18

1313

13 Fuse holder .......................................4,18

1414

14 RS232 interface......................................4

1515

15 Connection for detector block ...............4

1616

16 Connection for service ...........................4

1717

17 Serial number.........................................4

1818

18 Inlet capillary for injector ...................6,24

1919

19 Mounting rail ................................6,33,37

2020

20 Column connection

capillary ..............................6,29,31,33,37

2121

21 Sample loop...........................................6

2222

22 Injection valve..........................6,24,33,37

2323

23 Aspirating tubing....................................6

2424

24 Coupling.................................................6

2525

25 Syringe tubing ........................................ 6

2626

26 PEEK coupling .............................6,29,37

2727

27 Connection capillary .........................6,24

2828

28 Filter unit PEEK ..................6,16,24,36,37

2929

29 Connection capillary .........................6,24

3030

30 Connection capillary ..............................6

3131

31 Purge valve........................................6,24

3232

32 Aspirating capillary.................................6

3333

33 Fastening screws...................................6

3434

34 Pump head......................................6,147

3535

35 Connection capillary ..............................6

3636

36 Connection capillary ..............................6

3737

37 Inlet capillary for

detector block ..............................6,33,37

3838

38 Detector block..............................6,33,37

3939

39 Suppressor module ..........................6,37

4040

40 Tubing cartridge ...........................6,36,37

4141

41 Contact pressure lever .................6,36,37

4242

42 Holding clamp.................................. 6,37

4343

43 Snap-action lever .........................6,36,37

4444

44 Pump drive ........................................6,37

4545

45 Mounting pin .....................................6,37

4646

46 Compression fitting ......... 15,16,29,31,36

4747

47 Compression fitting ..............................15

4848

48 Capillary......................................15,16,31

4949

49 Connector with filter..............................16

5050

50 Housing for filter unit PEEK..................16

5151

51 Connector without filter ........................16

5252

52 Pulsation dampener .............................24

5353

53 Connection to injection valve ...............24

5454

54 Connection to purge valve ...................24

5555

55 Inlet capillary.........................................29

5656

56 Manufit housing....................................29

5757

57 PTFE gasket .........................................29

5858

58 2 Steel meshes.....................................29

5959

59 Precolumn cartridge.............................29

6060

60 Manufit pressure screw........................29

6161

61 Outlet capillary......................................29

6262

62 End fitting .............................................31

6363

63 Sleeve for precolumn cartridge............31

6464

64 Precolumn cartridge.............................31

6565

65 Connection piece .................................31

6666

66 Separating column.....................29,33,37

6767

67 Column holder.................................33,37

6868

68 Aspirating tubing for H2O ................36,37

6969

69 Aspirating tubing for H2SO4.............36,37

7070

70 Coupling ..........................................36,37

7171

71 Pump tubing for H2SO4...................36,37

7272

72 Pump tubing for H2O.......................36,37

7373

73 Stopper................................................ 36

7474

74 Coupling ......................................... 36,37

7575

75 Suppressor inlet capillary

for eluent......................................... 37,40

7676

76 Suppressor outlet capillary

for eluent......................................... 37,40

7777

77 Suppressor inlet capillary

for H2O....................................... 36,37,40

Table of contents

792 Basic IC

VIII

7878

78 Suppressor inlet capillary

for H2SO4....................................36,37,40

7979

79 Suppressor outlet capillary

for H2O ............................................37,40

8080

80 Suppressor outlet capillary

for H2SO4.........................................37,40

8181

81 Screw ................................................. 147

8282

82 Zircon piston ...................................... 147

8383

83 Spring retainer ................................... 147

8484

84 Spring................................................. 147

8585

85 Piston cartridge.................................. 147

8686

86 Piston guide sleeve............................ 147

8787

87 Sapphire supporting ring................... 147

8888

88 Piston guide sleeve............................ 147

8989

89 Piston seal ......................................... 147

9090

90 Inlet valve ....................................147,149

9191

91 Outlet valve..................................147,149

9292

92 Screw holder ......................................147

9393

93 Special tool ........................................147

9494

94 Special tool ........................................147

9595

95 Valve housing.....................................149

9696

96 Sealing ring ........................................149

9797

97 Sleeve.................................................149

9898

98 Sapphire sleeve .................................149

9999

99 Sapphire sphere.................................149

100

100100

100 Ceramic holder...................................149

101

101101

101 Seal ....................................................149

102

102102

102 Screw nut ...........................................153

103

103103

103 Connection piece...............................153

104

104104

104 Suppressor rotor ................................153

105

105105

105 Suppressor holder .............................153

1.1 Instrument description

792 Basic IC

1 Introduction

1.1 Instrument description

The 2.792.0020 Basic IC with suppressor module is a PC-controlled

system for ion chromatographic analyses. The extremely compact

housing of the 792 Basic IC contains everything needed to carry out ion

chromatography at a high quality level:

x Injection valve – for individual injections

x 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)

x 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

x Columns – whether anion columns with or without suppression,

separation columns for cations or organic acids – the 792 Basic IC

can accommodate them all

x Suppressor – integrated Metrohm Suppressor Module (MSM),

pressure-resistant, with fully automatic regeneration, highest per-

formance and optimal reproducibility

x 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

x Detector – conductivity detector with outstanding temperature

stability. The detector temperature of 40 °C varies by less than

0.01°C.

All components, which come into contact with eluent and sample are

metal-free.

The operation of the 792 Basic IC takes place via a PC connected to

the RS232 interface with the help of the control and evaluation program

«792 Basic IC». This PC program can be used to open prepared sys-

tems for recording and evaluating chromatograms and modify them if

need be. Time programs can also be created in which a large number

of instrument functions can be triggered for each program step.

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