CH-9101 Phone Fax Herisau/Switzerland ++41 71 353 85 85 ++41 71 353 89 01 Internet www.metrohm.com E-Mail info@metrohm.com 792 Basic IC Program «792 PC Software 1.0» 792 Basic IC Basic POWER 8.792.1003 Instructions for Use 11.04.
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..........................................................
Table of contents 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 ........................................
Table of contents 792 Basic IC 4.4 Methods ................................................................................................................. 80 4.4.1 Method file handling ............................................................................. 80 4.4.2 Passport................................................................................................ 80 General ......................................................................................... 81 Sample....................
Table of contents 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.....
Table of contents 6 Appendix .............................................................................................................. 159 792 Basic IC 6.1 Technical data.....................................................................................................159 6.1.1 Conductivity measurement................................................................. 159 6.1.2 Conductivity detector.......................................................................... 159 6.1.
Table of contents List of figures VI 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.
Table of contents List of numbered parts and controls 1 Door to interior ....................................3,6 40 Tubing cartridge ...........................6,36,37 2 Mains pilot lamp.....................................3 41 Contact pressure lever .................6,36,37 3 Feedthrough for syringe tubing .............3 42 Holding clamp.................................. 6,37 4 Feedthrough for aspirating tubing.........3 43 Snap-action lever .........................
Table of contents VIII 91 Outlet valve..................................147,149 92 Screw holder ......................................147 93 Special tool ........................................147 94 Special tool ........................................147 95 Valve housing.....................................149 Screw ................................................. 147 96 Sealing ring ........................................149 82 Zircon piston ......................................
1.1 Instrument description 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.
1 Introduction The operating software for the 792 Basic IC meets all the requirements you could place today on a modern integration software: single or multipoint 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, batch reprocessing; a powerful and GLP-conform report generator with outp
1.2 Parts and controls 1.2 Parts and controls 792 Basic IC Basic POWER 1 2 3 4 Fig. 1: Front of the 792 Basic IC 1 Door to interior 3 Feedthrough for syringe tubing for connection of the 6.2816.
1 Introduction 5 6 7 6 5 8 8 Waste B Waste A 9 8 8 17 Transport security screws 10 Type WARNING - Fire Hazard - For continued protection replace only with the same type and rating of fuse 16 f = 50-60 Hz S = 100 VA Service only Detector Block Fuse 100-120V: 1,0A(T) 220-240V: 0,5A(T) RS 232 Made by Metrohm Herisau Switzerland 11 12 13 15 14 Fig.
1.2 Parts and controls 5 Opening for detector cable 12 Mains connection plug mains connection, see section 2.4 6 Opening for outlet capillaries for discharge of eluent, regeneration solution, and rinsing solution from the inner compartment 13 Fuse holder changing the fuses, see section 2.
1 Introduction 38 37 1 36 35 18 19 20 21 34 39 33 32 31 19 22 40 30 41 POWER 23 24 29 28 27 Fig. 3: 6 26 45 44 25 43 42 Interior of the 792 Basic IC (with permanently attached accessories and 1.733.
1.2 Parts and controls 1 Door to interior 32 Aspirating capillary Connection for 6.1834.010 aspirating tubing 18 Inlet capillary for injector PEEK capillary, length L = 24 cm 33 Fastening screws for pump head 34 19 Mounting rail for 6.2027.0X0 column holder 34 Pump head (6.2824.100) 20 Column connection capillary PEEK capillary, length L = 30 cm 35 Connection capillary Connection pump head – purge valve, fixed mounting 21 Sample loop 20 PL 6.1825.
1 Introduction 1.3 Information on the Instructions for Use Please read through these Instructions for Use carefully before you put the 792 Basic IC into operation. The Instructions for Use contain information and warnings to which the user must pay attention in order to assure safe operation of the instrument. 1.3.1 Organization These 8.792.
1.3 Information on the Instructions for Use 1.3.2 Notation and pictograms The following notations and pictograms (symbols) are used in these Instructions for Use: Range SYSTEM STATE Menu item, parameter or entry value Program window Button [ Ctrl ] Key 35 Part or control of 792 Hazard This symbol draws attention to a possible danger to life or of injury if the associated directions are not followed correctly.
1 Introduction 1.4 Safety notes 1.4.1 Electrical safety While electrical safety in the handling of the 792 Basic 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: x 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.
2.1 Overview 2 Installation 2.1 Overview 2.1.1 Flow chart The following flow chart provides an overview of all installation work. You will find more detailed information in the relevant sections. Setting up sect. 2.2 Installing accessories sect. 2.3 Mains connection sect. 2.4 Connecting PC sect. 2.5 Connecting high pr. pump sect 2.6 Precolumn Yes No Installing sample loop Connecting column Suppressor Precolumn with twin cartridge holder sect. 2.7.2 sect. 2.7.3 Precolumn cat.
2 Installation 20 36 35 18 66 37 38 21 22 34 Detector Column 32 28 27 Injection valve 29 31 23 6.1834.010 25 30 52 24 6.2821.090 Waste Sample Eluent Fig. 4: Connecting diagram for 792 Basic IC without suppressor 20 36 18 35 66 75 76 26 37 21 22 34 Detector Column 32 79 78 29 31 23 30 39 77 80 28 27 6.1834.010 38 28 71 69 52 25 24 70 68 72 74 6.2821.090 Eluent Sample H2SO4 H2O Waste Fig.
2.2 Setting up the instrument 2.2 Setting up the instrument 2.2.1 Packaging The 792 Basic IC is supplied together with the separately packed accessories in special packagings containing shock-absorbing foam linings designed to provide excellent protection. The instrument itself is packed in an evacuated polyethylene bag to prevent the ingress of dust. Please store all these special packagings as only they assure transport of the instrument free from damage. 2.2.
2 Installation x Insert the cable permanently attached to the detector block 38 in one of the openings 5 and the outlet capillary in one of the openings 7 of the rear panel 9. x Replace rear panel 9 and screw to the 792 Basic IC using the four knurled screws 8. 2.3.
2.3 Attaching the accessories 2.3.4 Connection 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).
2 Installation 2.3.5 Filter unit PEEK One 6.2821.100 Filter unit PEEK (see Fig. 7) is already installed between the high-pressure pump and the injection valve 22 at the 792 Basic IC. This filter unit serves to avoid contamination by abrasive particles of the piston seals. The two other filter units PEEK supplied with the 792 Basic IC are installed between the pump tubings of the peristaltic pump and the inlet capillaries for regeneration and rinsing solution (see section 2.8.2).
2.4 Mains connection 2.4 Mains connection Follow the instructions below for connecting to the power supply. If the instrument is operated with a mains voltage set wrongly and/or wrong mains fuse, there is a danger of fire! 2.4.1 Setting the mains voltage Before switching on the 792 Basic IC for the first time, check that the mains voltage set on the instrument (see Fig. 8) matches the local mains voltage.
2 Installation 220 – 240 V 100 – 120 V 11 11 Mains switch 12 100 - 120 V 220 - 240 V 220 - 240 V 13 12 Mains connection plug 13 Fuse holder 100 - 120 V Fig. 8: Setting the mains voltage 2.4.2 Fuses 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 13 of the 792 Basic IC as standard.
2.5 Connection to the PC 2.5 Connection to the PC 2.5.1 Connecting cable Always switch off 792 Basic IC and PC before you connect the two instruments with the 6.2134.100 Cable. Connect the RS232 interface 14 at the 792 Basic IC to one of the serial COM ports at the PC using the 6.2134.100 Cable (9 pin/9 pin). If only a 25-pin COM interface is available on the PC then the optionally available 6.2125.110 Cable (9 pin/25 pin) or a commercially available adapter must be used. 2.5.
2 Installation 2.5.3 Basic settings When the program is started for the first time several basic settings must be made for the 792 Basic IC. Proceed as follows: 1 Start program x Double-click the software icon to start the program. The program window with the opening picture is opened and the Log In window appears on the screen: x Do not enter any password here, just click on . The following window appears: x Enter company, division and name and click on .
2.5 Connection to the PC x Click on COM1 using the right mouse button and select the Change menu item to open a window listing all available COM ports at the PC. x Select the desired COM port to which the 792 Basic IC has been connected and click on . The window is closed. x Close the Links window by clicking on . 3 Open a system x Click on File / Open / System in the main window. Open the folder Default. Select the system file Default.smt and click on .
2 Installation 4 Hardware settings Of the general hardware settings only the input of the cell constant is described. Standard settings can normally be used for all other parameters. x Click the 792 icon using the right mouse button and select the Hardware item. The Hardware settings window is opened: x In the Cell constant field enter the cell constant which is printed on the 1.732.0110 Detector block (see section 2.3.1). x Click on to close the window and save the settings.
2.6 High-pressure pump 2.6 High-pressure pump In order to avoid damage to the pump it must never be operated dry. Each time that the pump is switched on always first check that the eluent supply has been connected up correctly and that sufficient eluent is present in the eluent bottle. 2.6.1 Removing the transport security screws In order to prevent the pump drive from being damaged during transport the pump head is fitted with three transport security screws 10 (see Fig. 2).
2 Installation 18 29 31 POWER 28 27 54 53 52 22 Fig. 9: Connection of the pulsation dampener (option) 24 18 Inlet capillary for injector PEEK capillary, length L = 24 cm 31 Purge valve 22 Injection valve 52 Pulsation dampener (6.2620.150) 27 Connection capillary PEEK capillary, length L = 13 cm 53 Connection to injection valve 28 Filter unit PEEK (6.2821.
2.6 High-pressure pump 2.6.3 Connecting the eluent bottle To connect the eluent bottle with the high-pressure pump, insert the supplied 6.1834.010 aspirating tubing (i.d. = 1.5 mm, e.d. = 2.5 mm, length = 2.5 m) into one of the openings 5 or 7 in the interior of the 792 Basic IC. Pull the aspirating tubing sufficiently far into the interior of the 792 Basic IC and push at least 5 mm of it onto aspirating capillary 32 (see Fig. 3) of the high-pressure pump (it may be necessary to use emery paper).
2 Installation 3 26 Set flow rate to 2 mL/min x Double-click the 792 icon in the system window to open the window for manual control of the 792 Basic IC (see below). x Set the flow rate to 2 mL/min in the Flow field. x Click to to send this value to the 792 Basic IC.
2.6 High-pressure pump 792 Basic IC 4 Deaerate pump x Make sure that the 6.1834.010 aspirating tubing for the highpressure pump has been immersed into the eluent. x Click the button for IC pump to switch on the highpressure pump. x Use the syringe connected to the purge valve 31 to aspirate air until eluent flows into the syringe. x Click the button for IC pump to switch off the highpressure pump. x Close the rotary knob on purge valve 31 by turning it in a clockwise direction (see Fig.
2 Installation 2.7 Precolumns and separating columns 2.7.1 General information on precolumns The use of easily exchangeable precolumns protects the separating columns and prolongs their lifetime. The precolumns available from Metrohm (see section 6.3.2) are either real precolumns or precolumn cartridges, which are used together with the 6.2821.050 Twin cartridge holder or the 6.2828.110 Precolumn cartridge holder. New IC precolumns are normally filled with solution and sealed at both ends.
2.7 Precolumns and separating columns 3 Rinse the precolumn x Place a beaker beneath outlet capillary 61. 61 x Switch on 709 IC Pump, rinse precolumn for ca. 10 min with eluent and then switch off 709 IC Pump. Column 46 61 60 57 58 59 58 57 56 55 20 Column connection capillary of injector 26 PEEK coupling (6.2744.120) 46 Compression fitting (6.2620.000) 55 Inlet capillary 56 Manufit housing 57 PTFE gasket (6.2821.010) 58 2 Steel meshes (6.2821.
2 Installation 2.7.3 Precolumn glass cartridges with cartridge holder The precolumn glass cartridge METROSEP Anion Dual 1 (6.1006.030) is inserted in the 6.2828.110 Precolumn cartridge holder as follows (see Fig. 11): 30 1 Insert cartridge x Remove end fittings 62 from sleeve 63. 63 x Insert precolumn cartridge 64 in sleeve 63 (mark flow direction of the column cartridge on sleeve, the column cartridge should always be operated in the same flow direction).
2.7 Precolumns and separating columns 20 46 63 62 64 62 65 Fig. 11: Installation of precolumn glass cartridges with cartridge holder 20 Column connection capillary from injector 63 Sleeve for precolumn cartridge 46 Compression fitting (6.2744.010) 64 Precolumn cartridge (6.1006.030) 48 PEEK capillary (6.1831.010) 65 Connection piece for connection precolumn – column 62 End fitting 2.7.4 IC anion precolumn SUPERSEP The 6.1009.
2 Installation 2.7.5 General information on separating columns New IC separating columns are normally filled with solution and sealed at both ends. Before the column is installed in the system, it must be ensured that this solution is freely miscible with the eluent used (check manufacturer's specifications). The IC separating columns and precolumns currently available from Metrohm are listed in section 6.3.2. A test chromatogram and an information leaflet is provided with each column.
2.7 Precolumns and separating columns x with IC anion precolumn SUPERSEP: Screw inlet end of separating column 66 (note flow direction) to the precolumn installed as described in section 2.7.4. 2 Rinse column x Place a beaker beneath the column outlet. x Open software window for manual system control. x If necessary, modify Flow rate to the value suited for the inserted separating column and click on to send this value to the 792 Basic IC.
2 Installation 2.7.8 Installation of the separating column with suppressor For operation of the 792 Basic IC with suppressor module, the IC separating column is first connected to the injector or precolumn. The connection to the suppressor module and the detector block is described in section 2.8. 34 1 Connect column to injector x Remove end caps from column 66.
2.8 Suppressor module 2.8 Suppressor module 2.8.1 General information on suppressor module The Metrohm Suppressor Module MSM for chemical suppression installed in the 2.792.0020 Basic IC comprises a total of 3 suppressor units which are in turn used for suppression, regenerated with sulfuric acid and rinsed with water. To record every new chromatogram under comparable conditions, work is normally carried out with freshly regenerated suppressor.
2 Installation x Press contact pressure lever 41 on both tubing cartridges down as far as it will go. x Insert the pump tubings 71 and 72 (6.1826.060) into each of the tubing cartridges as shown in Fig. 13. The white-yellow stopper 73 must click into the corresponding holder on the left-hand side of the tubing cartridge. x Place the tubing cartridges on mounting pin 45 and press down on the right-hand side until snap-action lever 43 clicks into position on holding clamp 42.
2.8 Suppressor module 37 38 75 26 19 67 76 66 39 19 67 80 79 69 68 22 40 77 20 78 41 70 70 42 43 45 28 74 28 74 44 71 72 Fig. 14: Installation of column with suppressor 19 Mounting rail for column holder 67 66 Separating column 20 Column connection capillary PEEK capillary (6.1831.010; 30 cm) 67 Column holder (6.2027.0X0) 22 Injection valve 68 Aspirating tubing for H2O 6.1803.020 PTFE tubing 26 PEEK coupling (6.2744.040) 69 Aspirating tubing for H2SO4 6.1803.
2 Installation 39 Suppressor module 74 Coupling (6.2744.110) 40 Tubing cartridge (6.2755.
2.8 Suppressor module 4 2.8.4 Connect aspirating tubing for H2O x Prepare aspirating tubing 68: 68 Cut a piece of the 6.1803.020 PTFE tubing to the required length (normally ca. 120 cm). x Insert one end of the aspirating tubing 68 into the rinsing solution storage bottle and tighten it so that the tubing is firmly held. x Insert the free end of aspirating tubing 68 into one of the openings 5 of the 792 Basic IC (see Fig. 2) and pull it sufficiently far into the interior. x Mount a coupling 70 (6.
2 Installation Eluent 75 H2SO4 78 76 Detector 1 2 75 Suppressor inlet capillary for eluent 76 Suppressor outlet capillary for eluent 77 Suppressor inlet capillary for H2O 78 Suppressor inlet capillary for H2SO4 79 Suppressor outlet capillary for H2O 80 Suppressor outlet capillary for H2SO4 3 Waste 80 77 H2O 79 Waste Fig. 15: Connections at suppressor module 40 5 Inlet capillary for H2O x Attach inlet capillary 77 marked with "H2O" of suppressor module 39 using a 6.2744.
2.9 Putting into operation 2.9 Putting into operation 2.9.1 Putting into operation without suppressor Before sample solutions can be injected at the 792 Basic IC (without use of the suppressor), the entire system must be tested for leaks and then conditioned with eluent until the baseline is stable. Proceed as follows: 1 System öffnen x Start the «792 Basic IC» PC program, if it has not already been started (see section 2.5.3). x Select File / Open / System in the main window.
2 Installation 2.9.2 4 Check for leaks x Check all capillaries and their connections between the highpressure pump and the detector block for escaping liquid. If eluent escapes anywhere, the appropriate compression fitting must be tightened further or changed.
2.9 Putting into operation 3 Start system x Make sure, that the aspirating tubing 6.1834.010 for the highpressure pump is immersed in the eluent. x Select Startup determination from the Control menu in the system window. The high-pressure pump and the peristaltic pump are started, at the same time, a chromatogram window is opened where the baseline is recorded continuously. The suppressor module is automatically switched to the next position every 20 min and conditioned in this way.
2 Installation 44 792 Basic IC
3.1 Requirements 3 Operating tutorial This section introduces you to the operation of the 792 Basic IC by means of a brief operating tutorial which describes the basic operating steps needed for the recording of an ion chromatogram using one of the system files supplied. The determination of the anionic content of a drinking water sample with the METROSEP Anion Dual 1 column is used as an illustrative example. Please note that the steps and parameter settings described apply only to this example.
3 Operating tutorial 3.2 Preparations Before you start this brief tutorial, the entire IC system must be correctly installed as described in section 2. In what follows, the most important points for the installation are described once again (for details, see the sections mentioned). 1 2 3 4 46 Install 792 Basic IC Setting up instrument section 2.2 Installing and connecting detector block section 2.3.1 Mounting syringe and aspirating tubing section 2.3.2 Mains connection section 2.
3.3 Calibration 3.3 Calibration After the complete IC system has been installed as described in section 3.2, the first calibration can be started. A standard solution is required for this; it should contain the substances to be determined in approximately the same concentrations in which they can be expected in the sample. In our example of drinking water determination using the METROSEP Anion Dual 1 column a 20 PL sample loop is used; this is filled with the following standard solution: 0.
3 Operating tutorial 6 Start determination Click on in the system window or select Start determination of the Control menu. A chromatogram window opens where the baseline is recorded continuously. The status bar of this window shows the message Measure(Baseline), beside this running time, analysis time, absolute conductivity and number of measuring points per second are displayed. The message Waiting for INJECT [792COM#] appears in the SYSTEM STATE window.
3.3 Calibration 9 Switch injection valve to "FILL" position Click on the button of the 792 icon in the system window to switch the injection valve to the "FILL" position. At the same time, the suppressor module is switched to the next position. 10 Fill sample loop Immerse the aspirating tubing 23 in the standard solution. Using the syringe fixed to syringe tubing 25, 25 siphon in ca. 1 mL standard solution.
3 Operating tutorial 13 Modify integration parameters Click on or select Integration from the Method menu in the main window to open the integration parameters window. If required (e.g. if the fluoride peak is not detected), change the time delay Delay before starting peak integration. Click on . The Integration parameters window is opened and the chromatogram is reintegrated.
3.3 Calibration Repeat this procedure for all other integration parameters until the result satisfies your expectations. Click on for each parameter change. Close the Integration parameters window with . 14 Modify peak allocation Click on or select Calibration / Components from the Method menu. The prepared table for the components fluoride, chloride, nitrite, bromide, nitrate, phosphate and sulfate is displayed below the chromatogram.
3 Operating tutorial the status line. Enter this value (rounded off if necessary) into the Time column. The optimized table could, for example, then appear as follows: 15 Start calibration Click the button in the component window. Click on .
3.3 Calibration Confirm Level 1 with . Click on in the Concentrations window. 16 Display calibration curves Click on in the Components window. Select the desired component in the Component field for which the calibration curve should be displayed (e.g. for chloride). Close the Component - chloride window with . Close the Components window below the chromatogram by clicking on . 17 Save chromatogram and method Close the chromatogram window.
3 Operating tutorial 3.4 Sample determination Following the calibration of the IC system as described in section 3.3 the first sample solution can be injected. 1 Start determination Click on or select Start determination of the Control menu in the system window. An empty chromatogram window opens where the baseline is recorded continuously. The message Initialisation [792 COM#] appears in the SYSTEM STATE window. Then the Edit sample description window is opened automatically.
3.4 Sample determination 5 Switch injection valve to "INJECT" position Click on the button of the 792 icon in the system window to switch the injection valve to the "INJECT" position. At the same time, the data recording is started automatically. The status bar of the chromatogram window shows the message Measure, the SYSTEM STATE window shows the message INJECT done [792COM#].
3 Operating tutorial 7 Report output Click on or select Make report of the Process menu in the main window. The Report Options window appears. Under Report destination, switch on the desired target option for report output. Under Items to report and More items to report, click all desired elements for the report output. Click on to start the report output to the selected target. 8 Print report Click on or select Print of the File menu in the main window.
4.1 Fundamentals of the operation 4 Operation This section describes the most important points concerning operation of the 792 Basic IC. For further details, please refer to on-line help in the PC program, which can provide you with required information rapidly and conveniently from any place in program. 4.1 Fundamentals of the operation 4.1.1 Starting/closing the program the the the the Start the «792 Basic IC» program Start the program Double-click this icon or the Metro792.
4 Operation 4.1.2 Glossary System The term “system“ is used to describe the combination of instrument settings, time program and processing method, which have been optimized for the specific separating column and the determination to be carried out with it. A system is used to start single determinations or determinations with the help of a sample queue. Systems are stored as system files (*.smt) in the Systems directory.
4.1 Fundamentals of the operation Integration Integration is to be understood as being the method for determining the peak area and peak height with the aid of approximate baselines. The integration algorithm included in the program is influenced by the integration parameters and the optionally programmable integration events, which are defined in the method. In addition, the integration can be manually corrected later with the aid of the peak editor.
4 Operation 4.1.4 Main window elements The elements of the main window 792 BASIC IC are the menu bar, the tool bar and the status bar, indicating prompts and logged-in user. Menu bar Toolbar Status bar Prompts, information 4.1.
4.1 Fundamentals of the operation Enable/disable peak editor mode View whole chromatogram Help Lock system Opened system 4.1.6 Overview of file types The following file types are produced by the «792 Basic IC» software: 792 Basic IC *.bar Batch reprocessing file This binary file contains data of the batch reprocessing queue. The *.bar file is stored automatically in the Data folder. *.
4 Operation 4.1.7 Context sensitive menus Some of the menu functions of the program windows are also accessible by clicking on the desired window or item and pressing the right mouse button. The pop up windows have different contents and functions depending on the selected active window or item type. 4.1.8 Keyboard and mouse functions The mouse can be used to carry out the normal program operating functions such as the selection of menu items and fields.
4.1 Fundamentals of the operation Only part of the chromatogram is on screen: [ Ctrl ] + [ right ] Moves one window right (without change of scale on X and Y axes). [ Ctrl ] + [ left ] Moves one window left (without change of scale on X and Y axes). [ Home ] Shows the beginning of a chromatogram (without change of scale on X and Y). [ End ] Shows the end of a chromatogram (without change of scale on X and Y). [ 0 (Zero) ] Adjusts a zero on the lowest level in the window. Cursor is active: 4.1.
4 Operation 4.2 Instrument and software settings 4.2.1 Fonts 792 BASIC IC / Options / Fonts This option allows the selection of fonts used by the system. 4.2.2 Font for dialog... Selection of font used for dialog boxes. Default setting: MS Sans Serif / Standard / 8 pt. Font for reports... Selection of font used for report output to the screen or printer. Default setting: Courier New / Standard / 10 pt. Font for tables... Selection of font used for data presentation in tables on the screen.
4.2 Instrument and software settings Enter user name, password and access level for all users. Don't forget to make one of the users an Administrator, otherwise this window will not open again. At the end, click on . After configuration of the security system the program prompts for the password every time the system starts. This user name stamps all methods, chromatograms and reports. It is possible at any time to change the user with the menu item 792 BASIC IC / Options / Lock system. 4.2.
4 Operation Data file overwrite Never Overwriting of chromatogram files: Chromatogram files cannot be overwritten. A modified chromatogram is saved as a new file with the file name number raised by 1. Ask The user is asked if the chromatogram should be overwritten. Always Chromatogram files are always overwritten without confirmation. If method changed Saving of method files: Don't ask to save The method file is not saved automatically. It can be saved only with File / Save / Method.
4.2 Instrument and software settings 4.2.4 Measuring priority Setting the priority of program execution. realtime means that the «792 Basic IC» program has the highest priority, normal means that all active programs have the same priority. Default colors for chromatographic windows (details see section 4.5.3). COM port 792 BASIC IC / Options / 792 Basic IC:COM1 This menu item opens the Links window for COM port (serial RS232 interface) selection and settings.
4 Operation 4.3 Systems The term “System“ describes the combination of instrument settings, time program and processing method which has been optimized for a specific separating column and the determination to be carried out with it. A system is used to start single determinations. Systems are stored as system files (*.smt) in the Systems directory. 4.3.1 System window A system window is opened with 792 BASIC IC / File / Open / System and the selection of the desired system file.
4.3 Systems 4.3.3 System functions Start/stop hardware and record baseline SYSTEM / Control / Startup hardware (Measure Baseline) Starting the hardware at the 792 Basic IC includes sending of System startup values, starting of the high-pressure pump and starting of the peristaltic pump. At the same time, the recording of the measurement signal using the method defined for the system is started.
4 Operation Ident User defined identifier (title) for the chromatogram to be displayed in the title bar of the chromatogram window and in the Chromatogram open window. Calibration level Calibration level (0 = sample; 1}n = calibration solutions). Info 1 / Info 2 Sample description. Volume Injected volume in PL. Dilution Dilution of the sample. Vial number Autosampler vial position to take sample from. Amount Sample amount.
4.3 Systems 4.3.4 PC icon The PC icon is one of the components of the system window. If the system is connected and this icon is clicked with the right mouse button, the following menu items appear: 4.3.5 Open Load the processing method linked to the system and open an empty chromatogram window. Setup Open PC setup window for selection of processing method: Processing method Directory and name of the method file (*.mtw) linked to the system.
4 Operation The colors of the watch window fields can be changed by clicking the fields with the right mouse button and selecting the menu item Choose color / .... 4.3.6 Instrument icon Menu options for instrument icon System disconnected System connected Injection valve in "INJECT" position System connected Injection valve in "FILL" position The instrument icon for the 792 Basic IC is one of the components of the SYSTEM window.
4.3 Systems Flow, mL/min Pressure max, MPa Pressure min, MPa Startup value for flow rate of the high-pressure pump. Entry range: 0.20 ... 2.50 mL/min Startup value for maximum pressure limit for high-pressure pump. Entry range: 0.0 ... 25.0 MPa Startup value for minimum pressure limit for high-pressure pump. Entry range: 0.0 ... 25.
4 Operation Valve Suppressor IC pump Peristaltic System startup values Flow, mL/min Pressure max, MPa Pressure min, MPa Injection valve Switch injection valve to "INJECT" position. Switch injection valve to "FILL" position Suppressor module Switch the suppressor module to the next position. The time since the last switching of the suppressor module is displayed in the field beside the button. High-pressure pump Start high-pressure pump.
4.3 Systems Time (1st column) Time at which program instruction is applied. Entry range: 0.0 ... 999.9 min If no time is entered, the program instruction is applied together with the last instruction with time entry. Command (2nd column) Program instruction (see List of program instructions). Parameter (3rd column) Parameter for program instruction (see List of program instructions). ENABLED Enable program start (a disabled program is not started). Add new program instruction.
4 Operation Configuration The Configuration tab in the system settings window contains configuration settings for the 792 Basic IC. Method Selection of the method with or without suppressor: With MSM method with suppressor Without MSM method without suppressor Suppressor Suppressor module: Automatic switching to the next position each time the injection valve is switched either to the Fill or to the Inject position.
4.3 Systems Flow correction Factor for correction of the difference between displayed and actual flow rate of the highpressure pump. Range: 0.9 ... 1.09 The flow correction is determined by measurement of the actual flow rate with the aid of a measuring cylinder as follows: Displayed flow rate Flow correction = Measured flow rate Cell constant Cell constant of the conductivity cell for correct display of the absolute conductivity. Enter the cell constant printed on the detector block into this field.
4 Operation Event Pump stop Hardware error Power on 4.3.7 Events for alarm stop: Pump stopped because pressure limits are exceeded. Hardware error detected at the 792 Basic IC (high-pressure pump, injection valve, or suppressor not working correctly). Temporary power failure at the 792 Basic IC. System state window The SYSTEM STATE window is automatically opened if a system is opened. It shows status and error messages for this system.
4.3 Systems Error messages 792 Basic IC Detection of hardware failed Bad connection between PC and 792 Basic IC or instrument switched off (check connecting cable or switch on instrument). E1 Program checksum wrong (call Metrohm service). E2 RAM faulty (call Metrohm service). E200 Invalid instrument adjustment (call Metrohm service). E237 Storage of configuration values failed (repeat last action; if error reappears, call Metrohm service).
4 Operation 4.4 Methods A method contains all information necessary for data acquisition, integration, peak evaluation and quantification. It can be considered as the chromatogram template, i.e. chromatogram without raw data. Methods are stored as method files (*.mtw) in the Methods directory. 35 prepared, write-protected methods are copied to this directory at program installation. Each system is linked to a method.
4.4 Methods General Tab General of the passport with general description of the method and determination. Ident Duration METHOD DATA Date/time Last update Calibration level User Detector Run 792 Basic IC User defined identifier (title) for the chromatogram to be displayed in the title bar of the chromatogram window and in the Chromatogram open window. Duration of the chromatogram in minutes. You can modify this value when the chromatogram is running.
4 Operation To reset the Run number press [Ctrl] [F8]. The Analysis number window is opened where the run number for the next run can be modified to the desired value. Batch X/Y: total number of started sample queues / current analysis number in the sample queue (read-only). Sample Tab Sample of the passport with sample information. Info 1 Info 2 Volume Dilution Vial number 82 First sample description (max. 256 characters). Second sample description (max. 256 characters). Injected volume in PL.
4.4 Methods Column Tab Column of passport with column information. Number ID Length Serial number of column (max. 256 characters). Internal diameter of the column in mm. Length of the column in mm. This parameter is used to calculate Linear flow. Packing material Column Particle size Void volume Column description (max. 256 characters). Particle size of the column in Pm. This value is used for the calculation of reduced theoretical plate height Reduced TP height. Void volume for the column in %.
4 Operation Eluent Tab Eluent of passport with eluent information. Eluent A Eluent B Eluent C Flow Pressure Temp. Description of eluent composition (max. 256 characters). Description of eluent composition (max. 256 characters). Description of eluent composition (max. 256 characters). Flow rate of the high-pressure pump in mL/min. The flow rate is used to recalculate the time axis into volumetric units.
4.4 Methods Method Log Tab Method Log of passport with GLP Log for the method. The Method Log displays all automatically produced GLP messages concerning modifications made on a method. In addition to these messages, freetext user comments can be entered. All this entries are stamped automatically with date and time of the entry. 792 Basic IC Add a new GLP comment. Text can be entered in the New comment window, date/time and logged-in user are automatically added.
4 Operation Data Log Tab Data Log of passport with GLP Log for the recorded chromatogram. Here a GLP message is automatically produced for every modification made on a recorded chromatogram. In addition to these messages, free-text user comments can be entered. All this entries are stamped automatically with date and time of the entry and cannot be cleared. 86 Add a new GLP comment. Text can be entered in the New comment window, date/time and logged-in user are automatically added.
4.4 Methods 4.4.3 Method setup 792 BASIC IC / Method / Method setup This menu item opens the Method setup window that includes the most common parameters for data acquisition and evaluation of the method and consists of the following tabs: General General information on determination. Processing Set actions that are performed when the chromatogram finishes. Math Parameters that are used for various types of calculations.
4 Operation Make report Close window Chromatogram directory If checked, report auto-printing will be performed on data acquisition ending. If checked, the window is closed automatically after the run (or sample queue) is finished. Directory where the current chromatogram is saved. Use the button to select a new directory. Math Tab Math of Method setup window with parameters that are used for various types of calculations.
4.4 Methods European Pharmacopoeia US Pharmacopoeia Void time/volume Calculation method None 1st component 1st peak Formula setting according to European Pharmacopoeia. Formula setting according to US Pharmacopoeia. Calculation of void time/void volume: Selection of the method for void time calculation: Manual entry in the Void time field. The peak corresponding to the first component is selected as a void time marker and its retention time replaces the previous value of the void time.
4 Operation 4.4.4 Integration 792 BASIC IC / Method / Integration This menu item opens the Integration parameters window that contains parameters and events for peak integration and consists of the following two tabs: Setup Integration parameters. Events Integration events. The «792 Basic IC» software includes a built-in automatic integration algorithm to detect peaks on the chromatographic curve and to evaluate them using calculated baselines.
4.4 Methods Setup Tab Setup of Integration parameters window with integration parameters. The two most important of these parameters for peak recognition are Width and Slope. If the signal-to-noise ratio of the chromatogram is high enough (e.g. 100:1 or higher), the integration algorithm is not too sensitive to changes in integration parameters. On the contrary, if the baseline noise is high, careful tuning of these parameters may be needed. Number of peaks Number of peaks detected (read-only).
4 Operation Min height Minimum height of peaks to be detected. Negative peaks If this option is enabled, negative peaks are also detected. Events Tab Events of Integration parameters window for definition of integration events. Integration events have a higher priority than integration parameters and are used for fine-tuning of the integration process. They should be used only in the case when problems cannot be solved by tuning a set of parameters from the integration parameters window.
4.4 Methods Time Start time for integration event in min. Event List box with integration events to be selected (see below). Integration events Disable detection Set this mode to stop detection of new peaks. If a peak is available at the moment of the event it is either terminated (down slope peaks) or rejected (upslope peaks). Enable detection Clear Disable detection mode. Set peak start Force the beginning of a new peak.
4 Operation 4.4.5 Calibration and quantification General information The aim of any chromatographic analysis is to answer the question "What components are present in the sample and what are their concentrations?". Two procedures are used to achieve this goal: the first step is called calibration, the second step includes quantification.
4.4 Methods Notations R Stands for response value, either area or height, depending on setting selected in the Calibration graphs window. V Sample Volume injected. D Dilution V' = V / D Adjusted volume of injected sample. A correction is made for the dilution coefficient. C Concentration of the component in the initial solution (before dilution). Q = C • V' Quantity of component, used for calibration curve construction. t Retention time.
4 Operation External standard calibration External standard calibration (absolute calibration) is a key way of calibration. Basically this procedure calculates the dependence of injected component's quantity versus area (or height) of the corresponding peak. This dependence is showed as a calibration plot with injected quantity along the Y axis and peak area (or height) along the X axis.
4.4 Methods 792 Basic IC Number Row number (read-only). Peak Number of the peak in the chromatogram that corresponds to the given component. If this field contains a 0, the peak number must be entered manually. Time Expected retention time of the component in the calibration run. After a new entry of the peak number the corresponding retention time is entered automatically as soon as this field is clicked on with the mouse. Wind.% Identification window of the component.
4 Operation Additionally, the Components table contains the following buttons: Add a new component (an empty column) to the component table. Delete the current component from the component table. Open the Peak identification window (see Identification). Open the Concentration table (see Concentration table). Open the component window with display of calibration curve and calibration parameters.
4.4 Methods Identification Reference peaks Other peaks Identification parameters. Identification parameter for reference components. Default is Height. Identification parameter for ordinary components. Default is Time. Retention units Choice of retention units. Default is min. Retention time Retention time. Updates expected retention times of components according to the current chromatogram. Worst case...
4 Operation Concentration table 792 BASIC IC / Method / Calibration / Concentrations Selecting this menu item or clicking on in the component table opens the Concentrations window with the concentration table containing concentrations of all components for all Calibration levels. Each calibration level corresponds to a sample used for calibration and to a point on the calibration curve. 100 Concentration units User defined units of concentration that will appear in the report.
4.4 Methods Add a new Calibration level to the concentration table. The following window appears: Create calibration level Number of calibration level to add. Fill level with concentration Concentration to be filled in for all components. Copy concentrations from level Number of calibration level from which concentrations are copied. Calibrate immediately Recalibration with new calibration levels.
4 Operation Calibration curve 792 BASIC IC / Method / Calibration / Graphs Selecting this menu item or clicking on in the component table opens the Component window. In this window the results of the calibration are shown for each component together with the calibration curve. The parameters for calculating the calibration curve can also be entered here. Calibration results and curve 102 Analytical expression A line above the calibration curve looking like Q = k3 xA3 + k2 xA2 + k1 xA + k0.
4.4 Methods Calibration points table This table contains the basic information used to construct the calibration curve: Level Number of Calibration level. Conc. Concentration of the current component in the calibration sample. It is taken from the concentration table. Area (or Height) Peak height or area of the current component, depending on calibration base. File File name of calibration chromatogram that stores data on the given calibration level.
4 Operation Base Base for calculations (Area or Height) in quantification and calibration procedures. Indicates, which parameter is to be used as a peak response. Reference channel Channel which is used to measure area or height (read-only). Formula for calibration function. There are six possible calibration dependencies for linear and nonlinear calibration curves.
4.4 Methods Indexes Fill Index field for components with zero index. Coefficients Recalculate all calibration coefficients for all components (performs re-calibration). Recalculate coefficient of the universal component. The aim of this action is to adjust the response factor of this component so, that the total amount of the injected components becomes equal to the declared value. This declared summary amount is entered into the Concentration field of the universal component for This run level. Coef.
4 Operation 4.4.6 Report output Report options 792 BASIC IC / Method / Report options 792 BASIC IC / Process / Make report The Report options window is divided into several regions that combine parameters for report output on their functionality and includes several different areas. The report output is started by clicking on .
4.4 Methods Sample information from the Sample tab of the passport. Sample SAMPLE Info 1: Info 2: Vial number: Volume: Dilution: Amount: Tap water from Application Laboratory Herisau, Switzerland 2 20.0 µl 1.00 1.0000 Column information from the Column tab of the passport. Column COLUMN: Size: Number: Part.size: 6.1005.320 Metrosep A Supp3 4.6 x 250 mm A106 9.0 µm Eluent information from the Eluent tab of the passport. Eluent ELUENT A: B: C: Flow: Temperature: Pressure: 1.7 mM NaHCO3 / 1.
4 Operation Comment User defined comment from the Comment tab of the passport. COMMENT Beispielmethode zur Wasserbestimmung. GLP Log Method and Data GLP messages from the Method Log and Data Log tabs of the passport. METHOD GLP LOG 13/04/2000 08:32:49 W. Terzer 04/05/2000 10:45:23 792 Basic IC 1.0 Apr 27 2000 14:05:01 DATA GLP LOG Analysing data of channel :Cond Time constant, ms: 100.00 Sigma: 0.0 Rejection difference: 1.
4.4 Methods Calibration parameters defined in the component window and on the Math tab of the Method setup window. Calibration defaults CALIBRATION Method: Response: Standard: External standard Area No IDENTIFICATION Reference peaks: Other peaks: Retention units: Height Time min Component table. Component table COMPONENT TABLE No Retention Window% 1 2 3 4 5 6 7 4.05 5.01 5.82 6.63 7.74 11.67 13.20 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Calibration results 792 Basic IC RF Conc. 1.660e+00 2.735e+00 4.
4 Operation Parameters of the data acquisition channel used. Channel table CHANNELS TABLE No Name 1 Cond # Name/Units 1 Cond uS/cm Units Input uS/cm Minimum Zero 1 -8388607 0 Noise 1.5 1.52e-05 RMS 52871.6 0.529 Maximum Range Coefficient 8388607 8.389e+01 PeakToPeak 512493.0 5.12 Noise Shift 1.000e-05 1.52 0 Drift/hour 4232.464 0.0423 Name Channel’s name. This text appears as Channel label in the chromatogram. Units Units of detector response (PS/cm).
4.4 Methods Peak table The following parameters can be selected for peak table output with determination results: Quantification method Selection of the method to calculate concentrations of components: Response normalization The method normalizes the sum of responses for all peaks of the chromatogram to the NORM factor entered in the Total % for normalization field: Ri% = NORM • Ri / Ri. All peaks are calculated and reported no matter whether they have been recognized or not.
4 Operation As long as no universal component is defined, only peaks with non-zero concentrations are listed. The peak table includes the following columns: number, retention time, height, area, response factor, relative concentration, relative concentration%, name Index This column reports retention indexes of identified components.
4.4 Methods component the summary for all unidentified peaks is presented as a single line. Calls up a box with a list of columns that can be included into the report (see Report elements). It is available only if Quantification method = Custom has been selected. Report all peaks Checkbox that includes all peaks irrespective of the concentration of the substance. Otherwise the report generator excludes lines with zero concentration of the component.
4 Operation Character set The two options Windows (ANSI) or DOS (ASCII) are available. These settings are essential for printing of non-English symbols (e.g. ö, ä, ü). Custom program Path and name of the program to be started after report output. This option enables to transfer the report to a database, an electronic table or another application for further processing. Report elements If Quantification method = Custom has been selected, the peak table can be customized on the user's choice.
4.4 Methods resolution Resolution R for two neighboring peaks is calculated as: R = (ti+1 - ti) / (w0.607i + w0.607(i+1)) where i and i+1 indexes refer to the neighboring peaks, and w0.607 stands for the peak width at 60.7 % of the peak height. effectivity, TP Effectivity for the peak in number of theoretical plates. The number of theoretical plates Ni per column for a chosen peak is calculated for a chromatographic peak by one of two formulas: Ni = 2 PI (ti • Hi / Ai)2, where PI = 3.1415926...
4 Operation raw concentration Absolute concentrations (raw quantity) of the components, calculated as Ci = Wi(Ri) / V' Total value for the column is the sum of concentrations for all components. concentration% Normalization of concentrations for all peaks using the NORM value entered in the Total % for normalization field (default setting 100%): Ci% = NORM • Wi(Ri) / Wi(Ri) Total value for the column equals NORM for the main table, and the sum of concentrations in the group for the group table. rel.
4.4 Methods The types of components are designated by a one-letter code: type R Reference component (used for peak identification). S Standard component. C Calibration standard in the case it is different from the quantification standard. ? Some points of corresponding peak are out of ADC or detector range – suspicious result. ! Component concentration is outside of minimum (min C) and maximum limits (max C), set in the component table.
4 Operation 4.5 Chromatograms 4.5.1 Chromatogram window The CHROMATOGRAM window is used to show a running or recorded chromatogram. Title bar Status bar Chromatogram The title bar of the chromatogram window contains buttons for minimizing, maximizing and closing the window. The window name consists of the elements "Ident (method name) chromatogram name". A star ( * ) at the end of the name indicates that the chromatogram has been changed since the last saving. The status bar contains two fields.
4.5 Chromatograms 4.5.2 Chromatogram file handling Open chromatogram 792 BASIC IC / File / Open / Chromatogram Load an existing chromatogram file (*.chw) from the Data directory and open the chromatogram window. The following window appears: Filename Selected Directory File window Filename (common wildcards as * and ? are possible). Number of selected chromatograms and their total size. Path name of the working directory.
4 Operation to add a single chromatogram to the selection already made. All selected items are painted. Directories Box with the list of directories. Allows to change the working directory defined in the method, if necessary. Chromatogram description A set of fields with the description of the current chromatogram. Selected fields from the passport are listed here. Load all selected chromatogram files (*.chw) and open each in its own window.
4.5 Chromatograms Export chromatogram 792 BASIC IC / File / Export / AIA file Export the selected chromatogram in the AIA format (Analytical Instrument Association) as CDF file (*.cdf). 792 BASIC IC / File / Export / Raw data to txt Export chromatographic raw data into an ASCII text file (*.txt). The following window appears: Represent raw data as Default units (float) Output of raw data: Y values are exported in default units for the channel (PS/cm).
4 Operation 4.5.3 Graphical representation Appearance 792 BASIC IC / View / Appearance This menu item opens the Appearance window. It determines the appearance of the chromatogram and consists of four tabs: Chromatogram axes Labels Select channel Colors Scaling of chromatogram axes. Settings for peak labels and baseline drawing. Select channels to be displayed (only available for multi-channel chromatograms). Color settings for chromatogram elements.
4.5 Chromatograms Response axis Y from Y to Tic marks Beginning of the window on Y axis. End of the window on Y axis. Plot axes labels and tic marks on Y axis with no, relative or absolute scaling. View all Set scales on X and Y axes so that the whole chromatogram is visible. Drift compensation Turns the chromatogram screen image so that the last and first points of the chromatogram are on the same level. This option is useful for gradient chromatograms.
4 Operation Show baseline and peaks Baselines are shown. Baseline marker Start and end of baselines are marked. Label always visible Label is shown always with zooming. How to draw chromatogram point every middle random Channel labels At start In corner Set all Normal chromatogram drawing with all raw data points. Chromatogram drawing with additional smoothing of raw data points. Fast chromatogram draw for slow PCs. Label for data acquisition channel.
4.5 Chromatograms Colors Tab Colors of the Appearance window with color settings parameters for chromatograms. this color is default Hair Background Axes Baseline AlterGround Channel 1...8 792 Basic IC Reset the selected element to the default color. Choose a new color for the selected element. An example of the chosen color is shown beside the button. Cursor's color. Background color. Axes and axes labels color. Baseline color. Alternative background color for Measure baseline option.
4 Operation Other graphical functions 792 BASIC IC / View / X full scale By selecting this menu item or pressing [ Ctrl ] + [ Home ] the X axis is scaled so that the chromatogram perfectly fits the window horizontally. 792 BASIC IC / View / Y full scale By selecting this menu item or pressing [ Ctrl ] + [ End ] the Y axis is scaled so that the chromatogram perfectly fits the window vertically.
4.5 Chromatograms 4.5.4 Peak editor Switching on/off the peak editor 792 BASIC IC / Process / Peak editor The peak editor mode is used for subsequent manual correction of the automatic integration for chromatogram peaks (see section 4.4.4). It can be used to select the most important points for the peak evaluation (start, end and top of peak, valley between peaks) and move them to the required position. If the peak editor mode is enabled, the vertical bar cursor appears in the chromatogram window.
4 Operation 792 BASIC IC / Peak / Select end point Move the cursor to the end of the nearest peak and select the peak. 792 BASIC IC / Peak / Select valley point Move the cursor to the valley of the two nearest peaks. 792 BASIC IC / Peak / Unselect peak Delete the selection. [–] Move a selected point (start, top, end, valley) to the cursor position. 792 BASIC IC / Peak / Move selected point [+] Merge two neighboring peaks into a single peak.
4.5 Chromatograms 4.5.5 Printing Page layout for printing 792 BASIC IC / File / Page layout The selection of this menu item or clicking on in the Report options window opens the Page layout window for page layout parameters. Length units inches centimeters Page margins Left Right Top Bottom Chromatogram plot size Width Height Calibration graph size Width Height 792 Basic IC Selection of length units. Inches. Centimeters. Selection of page margins. Left margin. Right margin. Top margin.
4 Operation Printer settings 792 BASIC IC / File / Printer setup By selecting this menu item the PRINT SETUP window is opened where printer, paper size and format can be defined. Print preview 792 BASIC IC / File / Preview By selecting this menu item the Preview window appears on the screen where the report is shown in the appearance formatted for the desired printer as defined in the Report options window.
4.5 Chromatograms Subtraction of a chromatogram 792 BASIC IC / Process / More / Subtract This menu item opens the Subtract chromatogram window allowing the subtraction of any opened chromatogram from the active, selected chromatogram. Select the chromatogram that should be subtracted, click on and then on 792 BASIC IC / View / View all.
4 Operation 4.6 Batch reprocessing Reprocessing is understood to be the subsequent reprocessing of a series of chromatograms which have been loaded in a queue (Batch reprocessing queue). For reprocessing according to a selected method the settings for calibration, integration, passport, appearance and report can be altered at will. A batch reprocessing queue is stored in a batch reprocessing queue file *.bar in the Data directory. 4.6.
4.6 Batch reprocessing 4.6.2 Perform batch reprocessing Reprocess options window 792 BASIC IC / File / Open / Batch reprocessing 792 BASIC IC / File / Open / Last batch These two menu items are used to open the Reprocess window, in which the various options for reprocessing are set and can then be triggered. Use method from file for reprocessing Selection of the desired chromatogram file whose method should be used for reprocessing.
4 Operation Open the batch reprocessing editor program for editing the batch reprocessing table (see section 4.7.3). Reprocess sample runs Reprocess all sample chromatograms (calibration level = 0). Reprocess calibration runs Reprocess all calibration chromatograms (cali- bration level > 0). Update method file in directory after reprocessing Save the method file *.mtw after reprocessing the method is changed.
4.6 Batch reprocessing Recalculate only Enable recalculation of chromatograms with values for Volume, Dilution, Amount and Internal standard amount entered in the batch reprocessing table. The recalculation is done automatically if the and/or Recalculate options are enabled. If the Recalculate only option is enabled, the Reintegrate and Recalculate options are disabled automatically.
4 Operation Merge chromatograms REPROCESS / Combine all chromatograms of the batch reprocessing queue into a single multi-channel chromatogram. The chromatograms are displayed in the same order as in the batch reprocessing table slightly displaced one upon the other. The distance between the curves can be increased by pressing [ Shift ] + [ n ] and decreased by pressing [ Shift ] + [ p ]. The chromatogram axes, labels and colors can be set in the Appearance window.
4.6 Batch reprocessing 4.6.3 Batch reprocessing queue editor Open batch reprocessing queue editor window REPROCESS / This menu item opens the batch reprocessing editor program for editing the batch reprocessing table. No Row number. File name Name of the chromatogram file (read-only). Method Name of the method file *.mtw used for recording the chromatogram (read-only). Ident User defined identifier for chromatogram.
4 Operation Sample Info 1 First sample description. Will be placed into appropriate passport field. Sample Info 2 Second sample description. Will be placed into appropriate passport field. Batch reprocessing queue editor functions The functions in the editor window for the batch reprocessing queues can be triggered with the corresponding menu items of the Edit menu or with the corresponding symbols in the symbol bar.
5.1 Practical notes on ion chromatography 5 Notes – Maintenance – Faults 5.1 Practical notes on ion chromatography 5.1.1 Separating columns Separation efficiency The attainable quality of analyses with the 792 Basic IC depends to a large extent on the separation efficiency of the column used. When purchasing an IC column you should ensure that the separation efficiency suffices for the analysis problems at hand.
5 Notes – Maintenance – Faults Storage Always store the separating columns closed when not in use and filled in accordance with the manufacturer’s specifications. Dead volume Dead volume at the end of a column can be the cause of extreme peak broadening or splitting (appearance of double peaks). Filling the column with glass beads ( d 100 Pm) frequently improves the separation efficiency.
5.1 Practical notes on ion chromatography 5.1.3 Eluents Treatment For the preparation of the eluents, only chemicals of a purity degree of at least "p.a." should be used. For diluting, please use only high purity water. Fresh eluents should always be microfiltered (0.45 Pm filter) and degassed (with N2, He or vacuum). For alkaline eluents and eluents with low buffering capacity one should preferably use a CO2 absorber.
5 Notes – Maintenance – Faults 5.1.5 Suppressor module Protection To avoid contamination of the suppressor module by foreign particles or bacterial growth, the two 6.2821.100 Filter units PEEK (see section 2.3.5) supplied must be installed between peristaltic pump and inlet capillaries of the suppressor module (see section 2.8.2). Operation The Metrohm Suppressor Module MSM comprises a total of 3 suppressor units which are in turn used for suppression, regenerated with sulfuric acid and rinsed with water.
5.2 Maintenance and servicing 5.2 Maintenance and servicing 5.2.1 General information Care The 792 Basic IC requires proper care and attention. Excessive contamination of the instrument could possibly lead to malfunctions and a shorter service life of the inherently rugged mechanical and electronic parts. Spilled chemicals and solvents should be wiped up immediately.
5 Notes – Maintenance – Faults 5.2.3 Recycling To keep the eluent consumption between injections to a minimum when the system is at rest (e.g. overnight), the so-called recycling procedure can be used. In recycling the eluent exiting the outlet capillary of the detector block is led back directly to the eluent supply vessel. The IC system is thus quickly ready for new injections without a long conditioning period.
5.2 Maintenance and servicing 3 Rinse column x Place beaker beneath the column outlet. x Switch on high-pressure pump and rinse column with eluent for ca. 10 min, then switch off pump. 4 Connect column to detector block x Screw outlet end of separating column 66 to inlet capillary 37 or suppressor inlet capillary 75. 75 Changing the separation system If you wish to replace an IC separating column by a column of a different type, proceed as follows (see Fig. 12 and Fig.
5 Notes – Maintenance – Faults 5.2.6 Maintenance work at the pump head In many cases, an unstable baseline (pulsation, flow fluctuations) can be traced to contaminated valves or faulty, leaky piston seals at the high-pressure pump. For cleaning contaminated valves and/or replacement of wear parts such as pistons, piston seals and valves, proceed as follows: 1 Detach pump head x Disconnect aspirating tubing from aspirating capillary 32 at the pump head 34 (see Fig. 3).
5.2 Maintenance and servicing 92 34 81 82 83 84 91 85 86 87 88 89 90 92 Fig. 16: Components of the pump head A 34 93 94 89 94 B 89 C 93 Fig. 17: Replacement of the piston seal 89 34 Pump head (6.2824.100) 88 Piston guide sleeve (4.709.4370) 81 Screw (3.709.1100) for piston cartridge 85 89 Piston seal (6.2741.020) 82 Zircon piston (6.2824.070) with piston shaft 90 Inlet valve (6.2824.090) 83 Spring retainer 4.709.0730 91 Outlet valve (6.2824.080) 84 Spring (6.2824.
5 Notes – Maintenance – Faults x To install a new piston seal 89 the special tool 94 is used. x First the new seal is inserted firmly in the recess of tool 94 by hand (see Fig. 17B). The seal spring must be located on the outside. x The tool 94 together with the seal is then inserted in the pump head 34 and the seal pressed into the pump head recess with the aid of tool 93 (see Fig. 17C).
5.2 Maintenance and servicing 6 Mounting the pump head x Reassemble the components of the pump head 34 as shown in Fig. 16. Tighten the screw 81 by hand. First screw in piston cartridge 85 manually until the stop is reached and then use a wrench to turn it through a further 15°. Firmly tighten the two valve screw holders 92 with a wrench. x Reattach pump head 34 to the pump with the help of the 4 fixing screws 33. 33 Firmly tighten them with the 6.2621.030 Allen key.
5 Notes – Maintenance – Faults 5.2.7 Regeneration of the suppressor module Regenerating a suppressor operating at reduced capacity If the suppressor units are exposed to certain heavy metals (e.g. iron) or organic contaminants for long periods, these can no longer be completely removed by the regeneration solution normally used (20 mmol/L H2SO4).
5.2 Maintenance and servicing x Set the flow at the high-pressure pump to 0.5 mL/min and rinse the suppressor unit with 1 mol/L H2SO4 for 5 to 10 min. x As the pressure falls, slowly increase the flow at the highpressure pump to 2 mL/min. Do not exceed a maximum pressure of 2 MPa (20 bar). x Switch off high-pressure pump. x Switch suppressor to the next position using the button. x Connect the inlet capillary 77 marked "H2O" to the inlet capillary 18 using coupling 26 (see Fig. 9 and Fig. 14).
5 Notes – Maintenance – Faults 152 2 Dismantle suppressor x Unscrew nut 102 from suppressor holder 105. 105 x Pull out connection piece 103 and suppressor rotor 104 from suppressor holder 105 (the connection piece and the rotor normally stick together). x Loosen connection piece 103 from suppressor rotor 104. 104 3 Clean input and output leads x Connect each of the 6 capillary tubings attached to connection piece 103 to the high-pressure pump one after another, and pump through ultrapure water.
5.2 Maintenance and servicing 102 103 104 105 Fig. 19: Assembling the suppressor 5.2.9 102 Screw nut 104 Suppressor rotor (6.2832.000) 103 Connection piece (6.2832.
5 Notes – Maintenance – Faults 154 3 Clean suppressor rotor x Clean the sealing surface of new suppressor rotor 104 (6.2832.000) using a lint-free cloth and ethanol. 4 Insert suppressor rotor x Insert new suppressor rotor 104 in suppressor holder 105 in such a way that the tubing connections at the rear of the rotor fit in the corresponding openings inside the rotor and that one of the three holes in the rotor can be seen from below in one of the openings of the holder.
5.2 Maintenance and servicing 5.2.10 Exchanging the pump tubing The pump tubings used by the peristaltic pump are consumable material with a limited lifetime and should be exchanged at regular intervals (approx. every 4 weeks under continuous use). The working life of pump tubing depends to a considerable extent on the contact pressure. This is why the contact pressure must be correctly set as described in section 2.9.2.
5 Notes – Maintenance – Faults 5.3 Faults and malfunctions 5.3.1 Error messages If any type of malfunction occurs during operation of the 792 Basic IC, this is shown by error messages in the PC program, which appear either in an error window or in the SYSTEM STATE window. Follow the instructions given in the error window and close this window with .
5.3 Faults and malfunctions 792 Basic IC Malfunction Cause Rectification Chromatograms with poor resolution, change in the retention times x Deterioration in separation efficiency of the IC column x Regenerate column (see section 5.1.
5 Notes – Maintenance – Faults 5.4 Diagnostic tests / Validation / GLP The requirements of GLP (Good Laboratory Practice) include a periodic check of analytical measuring instruments with regard to their reproducibility and accuracy using Standard Operating Procedures, SOP. Under the title «Application Bulletin No.
6.1 Technical data 6 Appendix 6.1 Technical data 6.1.1 Conductivity measurement 6.1.2 Measurement range 0}1000 PS/cm (resolution: 0.56 nS/cm) Maximum error r 10 PS/cm and r 1 % of measurement value (k = 16.7/cm) Linearity Deviations < r 5 PS/cm Noise typ. 3 nS/cm Drift (electronic) typ. < 10 nS/cm / h Temperature dependence typ. < 40 nS/cm / °C Reserve range > 33 % (k = 16.
6 Appendix 6.1.3 6.1.4 Injection valve Actuator switching duration 100}150 ms Pressure resistance 25 MPa (250 bar) High-pressure pump Type Serial dual piston pump with two valves Pump capacity Flow range Maximum error Flow constancy Reproducibility of eluent flow 0.20...2.5 mL/min < r 2 % of set value < 0.5 % of set value typ. better than r 0.
6.1 Technical data 6.1.5 Peristaltic pump Type Pump capacity Rotational speed Flow range Maximum error 6.1.6 6.1.7 2-channel peristaltic pump 20 U/min at 50 Hz 24 U/min at 60 Hz 0.5}0.6 mL/min with 6.1826.060 Pump tubing r5% Maximum pressure 0.4 MPa (4 bar) Pumpable liquids Clear liquids with no solid contents Pump tubing material PP (polypropylene) Suppressor module Switching duration 140 ms Pressure resistance 2.
6 Appendix 6.1.8 6.1.9 6.1.10 162 Mains connection Voltage 115 V: 100...120 V r 10 % 230 V: 220...240 V r 10 % Frequency 50...60 Hz Power consumption 100 VA Fuse 5 mm dia., 20 mm length 100}120 V: 1.0 A (slow-blow) 220}240 V: 0.
6.1 Technical data 6.1.11 6.1.12 792 Basic IC Ambient temperature Nominal operating range +5}+45°C (at 20}80 % atmospheric humidity) Storage –20}+70°C Transport –40}+70°C Housing Material of cover Polyurethane rigid foam (PUR) with fire protection for fire class UL94VO, CFC-free Material of base Steel, enameled Width 255 mm Height 385 mm Depth 343 mm Weight (incl. accessories) 15.
6 Appendix 6.2 Standard equipment Subject to changes ! All dimensions are given in mm. The 2.792.0020 Basic IC includes the following parts: Quant. Order No. Description 1 1.732.0110 Detector block (metal-free) with permanently attached connecting cable to 792 Basic IC 1 6.1803.020 PTFE capillary Length = 5 m 2 1 6.1826.060 6.1834.010 0.97 1.57 1.5 2.5 150 Pump tubing made of PP (polypropylene) with 2 firmly attached white-yellow stoppers; in.d. = 0.51 mm, ex.d. = 2.
6.2 Standard equipment Quant. Order No. Description 1 6.2617.010 Special tool For removing the piston seal of the pump head M3.5 35 1 6.2621.030 50 Hexagon key 4 mm For mounting the pump head of the high-pressure pump. 73 29.5 2 6.2744.010 PEEK compression fitting For the connection of 6.1831.010 PEEK capillaries or 6.1822.010 PTFE microcapillaries, set of 5 26 1 1 6.2744.030 6.2744.040 PEEK coupling Connection between 6.2744.010 PEEK compression fitting and 6.1826.
6 Appendix Quant. Order No. Description 2 6.2821.100 Filter unit PEEK 2 Pm To avoid contamination due to abrasive particles of piston seals. 16 Spare part: 6.2821.110 Filter 25.5 166 1 6.6045.003 Software-CD «792 Basic IC 1.0» 1 Y.107.0150 Cable strap 1 8.732.2003 Metrohm Monograph «Ion chromatography» (English) 1 8.732.2013 «IC Application Notes» (English) 1 8.792.1003 Instructions for Use (English) for 792 Basic IC 1 8.792.
6.3 Optional accessories 6.3 Optional accessories 6.3.1 Accessories for 792 Basic IC Order No. 6.1825.XXX Description Sample loop, made of PEEK For injection valve; incl. two 6.2744.010 PEEK compression fittings 6.1825.230: Volume = 6.1825.210: Volume = 6.1825.220: Volume = 6.1831.010 6.2620.150 10 PL 20 PL 100 PL PEEK capillary Length = 3 m Pulsation dampener MF Metal-free pulsation dampener to reduce pulsation and prolong the life of separating columns. 0.25 e16" 1 52 76 6.2621.
6 Appendix Order No. 6.2824.050 Description Spring for main piston Spare part for 6.2824.100 Pump head 11 30 6.2824.060 Spring for auxiliary piston Spare part for 6.2824.100 Pump head 11 47 6.2824.070 Zircon piston Spare part for 6.2824.100 Pump head 3 65.5 6.2824.080 Outlet valve (metal-free) 8 Spare part for 6.2824.100 Pump head 16 6.2824.090 Inlet valve (metal-free) 8 Spare part for 6.2824.100 Pump head 16 6.2824.100 Pump head (metal-free) Complete, with fixations screws 6.5324.
6.3 Optional accessories 6.3.2 Separating columns and precolumns Order No. Description 6.1005.000 IC anion column PRP-X100 (125 mm) For the determination of anions without chemical suppression. Column dimensions: 125 u 4.0 mm Precolumn: 6.1005.020 6.1005.010 IC anion column PRP-X100 (250 mm) For the determination of anions without chemical suppression. Column dimensions: 250 u 4.0 mm Precolumn: 6.1005.020 6.1005.020 IC precolumn cartridge PRP-X100 To prolong the service life of 6.1005.000 and 6.
6 Appendix Order No. Description 6.1005.300 IC anion column METROSEP A SUPP 1 For the determination of anions with chemical suppression. Column dimensions: 250 u 4.6 mm Precolumn: 6.1011.020 6.1005.310 IC anion column METROSEP A SUPP 2 For the determination of anions with chemical suppression. Column dimensions: 250 u 4.6 mm Precolumn: 6.1011.020 6.1005.320 IC anion column METROSEP A SUPP 3 For the determination of anions with chemical suppression. Column dimensions: 250 u 4.6 mm Precolumn: 6.1011.
6.3 Optional accessories Order No. Description 6.1006.200 Preconcentration cartridge METROSEP Anion For anion preconcentration. Column dimensions: 30 u 3.1 mm Installation using 6.2828.110 Precolumn cartridge holder. 6.1006.300 Preconcentration column METROSEP Anion For anion preconcentration. 6.1006.430 IC anion column METROSEP A SUPP 4 For the determination of anions with chemical suppression. Column dimensions: 250 u 4.0 mm Precolumn: 6.1006.500 Note: The 6.2620.
6 Appendix Order No. Description 6.1007.000 IC cation column Nucleosil 5SA For the determination of divalent cations without chemical suppression. Column dimensions: 125 u 4.0 mm Precolumn: 6.1007.010 6.1007.010 IC precolumn cartridge Nucleosil 5SA To prolong the service life of the 6.1007.000 IC cation column Nucleosil 5SA. Column dimensions: 20 u 4.0 mm Installation using 6.2821.050 Twin cartridge holder. 6.1008.
6.3 Optional accessories Order No. Description 6.1010.200 IC precolumn METROSEP C 2 Guard To prolong the service life of the METROSEP C 1 and C 2 cation columns. 6.1010.210 IC cation column METROSEP C 2 100 For the determination of monovalent and divalent cations without chemical suppression. Column dimensions: 100 u 4.0 mm Precolumn: 6.1010.200 6.1010.220 IC cation column METROSEP C 2 150 For the determination of monovalent and divalent cations without chemical suppression.
6 Appendix Order No. Description 6.1012.X20 Sample pretreatment cartridge IC-Ag Cation exchanger in Ag+ form. Removes halides. With Luer connection. 6.1012.020: set of 50 6.1012.120: set of 10 6.1012.X30 Sample pretreatment cartridge IC-OH Cation exchanger in OH– form. For highly acidic samples. With Luer connection. 6.1012.030: set of 50 6.1012.130: set of 10 6.1012.200 Sample pretreatment cartridge Chromafix C18 Removes organic substances (not suitable for fluoride determinations).
6.3 Optional accessories 6.3.3 Order No. Description 6.2828.120 Glass cartridge holder To hold the 6.1006.0040 Column cartridge METROSEP Anion Dual 1. 6.2832.000 Suppressor rotor Replacement cartridge for Metrohm suppressor module. 6.2832.010 Connection piece for suppressor rotor with input and output leads Additional devices and cables Order No. Description 6.2125.010 Cable Connecting cable 792 Basic IC (RS232 interface) – PC Adapter cable 25-pin to 9-pin. 9 pol. neg. 25 pol. 0.3 m 6.2125.
6 Appendix 6.4 Warranty and conformity 6.4.1 Warranty The warranty on our products is limited to defects that are traceable to material, construction or manufacturing error that occur within 12 months from the day of delivery. In this case, the defects will be rectified in our workshops free of charge. Transport costs are to be paid by the customer. For day and night operation, the warranty is limited to 6 months. Glass breakage in the case of electrodes or other parts is not covered by the warranty.
6.4 Warranty and conformity 6.4.2 EU Declaration of conformity EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies, that the instrument: 792 Basic IC meets the requirements of EC Directives 89/336/EEC and 73/23/EEC.
6 Appendix 6.4.3 Certificate of conformity and system validation Certificate of Conformity and System Validation This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. Name of commodity: 792 Basic IC System software: Stored in ROMs Name of manufacturer: Metrohm Ltd.
6.5 Index 6.5 Index 1 1st component ...................................... 89 1st peak................................................. 89 7 792 BASIC IC .................................... 59,60 A Abrasive particles ............................... 140 Absolute calibration....................... 96,103 Absolute concentration ................ 111,116 Access levels........................................ 64 Accessories for 792 Basic IC .............................. 167 High-pressure pump ..............
6 Appendix Cell constant ..................................77,159 Entry .................................................. 22 Printed ............................................... 13 Cell volume ......................................... 159 Ceramic holder 100 Figure .............................................. 149 Certificate of conformity and system validation ............................ 178 Change passport ................................. 135 Changing of separating column......................
6.5 Index Coupling 74 Connect pump tubing ...................... 36 Figure........................................... 36,38 Ordering designation ..................... 165 Create calibration level ....................... 101 Cursor ................................... 125,127,128 Custom................................................ 112 Custom formulae................................... 88 Custom program ................................. 114 ....................................... 113 D DATA ...
6 Appendix Glass cartridge holder (6.2828.100).................................... 174 Glass cartridge holder (6.2828.120).................................... 175 Global preferences ................................ 65 Global settings ...................................... 65 Glossary ................................................ 58 GLP ...............................66,85,86,108,158 GLP comment.................................. 85,86 GLP Log ....................................85,86,108 GLP messages ....
6.5 Index Interpolation .......................................... 89 Introduction..............................................1 Invert! .................................................. 131 Ion chromatography........................... 139 Items to report..................................... 106 K Keyboard ....................................... 62,128 Knurled screw 8 Figure...................................................5 Open rear panel ............................... 13 L Label always visible ...
6 Appendix Outlet capillary 61 Figure ................................................ 29 Installation ......................................... 28 Outlet valve 91 Cleaning .......................................... 148 Components ................................... 149 Figure .......................................147,149 Ordering designations .................... 168 Replacement................................... 148 Overview File types........................................... 61 Program windows .......
6.5 Index Figure........................................... 36,37 Installation......................................... 35 Ordering designation ..................... 164 Set contact pressure ........................ 43 Working life .............................. 141,155 Purge valve 31 Dearate pump .................................. 25 Figure............................................. 7,24 Putting into operation with suppressor ................................ 42 without suppressor.........................
6 Appendix Separating column 66 Changing ........................................ 144 Characteristic data.......................... 139 Connection at detector block 38 ............................................ 33 Connection to suppressor module 39......................................... 39 39 Dead volume................................... 140 Figure ........................................... 33,37 Fixing............................................ 33,34 General information ..........................
6.5 Index Total % for normalization .................... 112 Transport .............................................. 13 Transport damage.............................. 176 Transport security screws 10 Figure...................................................5 Remove ............................................ 23 Treatment of eluents........................... 141 Tubing cartridge 40 Figure........................................ 7,36,38 Install pump tubings......................... 35 Raise...............
6 Appendix 188 792 Basic IC
