Metrohm Ltd. CH-9101 Herisau/Switzerland Phone ++41 71 353 85 85 Fax ++41 71 353 89 01 Internet www.metrohm.ch E-Mail info@metrohm.ch 6.6034.003 Metrodata IC Net 2.0 8.110.8193 Software Manual 25.01.
All Rights Reserved.
Table of contents Table of contents 1 Introduction .......................................................................................... 1 1.1 1.2 1.3 1.4 2 Fundamentals of the operation.............................................. 5 2.1 2.2 2.3 2.4 2.5 2.6 2.7 2.8 2.9 3 Fonts ............................................................................................13 Security system ..........................................................................13 Global settings..................
Table of contents 4.3 4.4 4.5 5 Interfaces ........................................................................................... 29 5.1 5.2 5.3 5.4 5.5 5.6 II System functions........................................................................20 4.3.1 Connect and disconnect system .................................20 4.3.2 Start/stop hardware and record baseline.....................21 4.3.3 Start/stop determinations.............................................22 4.3.
Table of contents 6 Devices ................................................................................................. 53 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8 6.9 6.10 6.11 IC Net 2.0 Device installation......................................................................53 6.1.1 Install devices at system creation ................................53 6.1.2 Install new devices in system window..........................54 6.1.3 Install existing devices in system window ....................54 6.
Table of contents 6.12 6.13 7 Methods................................................................................................ 99 7.1 7.2 7.3 7.4 7.5 7.6 IV Data recorder ..............................................................................96 6.12.1 Data recorder icon .......................................................96 6.12.2 Select processing method and data source................96 System timer ...............................................................................
Table of contents 8 Chromatograms .......................................................................... 145 8.1 8.2 8.3 8.4 8.5 8.6 9 Sample queue ............................................................................... 163 9.1 9.2 9.3 IC Net 2.0 Chromatogram window .......................................................... 145 Chromatogram file handling .................................................. 146 8.2.1 Open chromatogram .................................................
Table of contents 10 Batch reprocessing .................................................................. 169 10.1 10.2 10.3 Batch reprocessing queue file handling .............................. 169 10.1.1 Open batch reprocessing queue ...............................169 10.1.2 Create new batch reprocessing queue......................169 10.1.3 Save batch reprocessing queue ................................170 Perform batch reprocessing .................................................. 170 10.2.
1.1 Purpose of program 1 Introduction 1.1 Purpose of program «ICNet 2.0» is the name of the data acquisition and control software for PC-controlled ion chromatographic systems consisting of Metrohm and Bischoff instruments. The current version is a true 32-bit application. It was designed specially to operate under Windows 95, Windows 98 and Windows NT and uses all its benefits. The «ICNet 2.0» program can be used to create systems for recording and evaluating chromatograms.
1 Introduction Section 5 Interfaces Installation, control and parameter settings of interfaces Section 6 Devices Installation, control and parameter settings of devices Section 7 Methods Method parameters, integration, calibration, quantification, report Section 8 Chromatograms Chromatogram appearance, peak editor Section 9 Sample queue Sample queue control and editor Section 10 Batch reprocessing Reprocessing of chromatograms Section 11 Appendix Software license, ordering designations, index To find the r
1.4 Installation Button [ Ctrl ] Key Hazard This symbol draws attention to a possible danger to life or of injury if the associated directions are not followed correctly. Warning This symbol draws attention to possible damage to instruments or instrument parts if the associated directions are not followed correctly. Caution This symbol marks important information. First read the associated directions before you continue. Comment This symbol marks additional information and tips. 1.
1 Introduction The two software packages «IC Net 2.0» and «Autodatabase 1.0» will be installed in the desired directory. Icons are created in the program folder, in the startup folder, and on the desktop. In addition to the program files of the «IC Net» program, the following folders are installed: 1.4.3 Data Folder for storage of chromatogram files (*.chw) and batch reprocessing files (*.bar) with several examples. Devices Folder for storage of device files.(*.dev).
2.1 Starting/closing the program 2 Fundamentals of the operation 2.1 Starting/closing the program 2.1.1 Start the «IC Net» program Start the program Double-click this icon or the ICNet.exe file to start the «IC Net 2.0» program. The IC Net login window appears: Enter your password and click on . After software installation, the program can be started without entering a Password. For the definition of users, see section 3.2. 2.1.
2 Fundamentals of the operation 2.2 Glossary Batch reprocessing Batch reprocessing is understood to be the subsequent reprocessing of a series of chromatograms which have been loaded in a batch reprocessing queue. During reprocessing with a selected method the settings for calibration, integration, passport, appearance and report can be altered at will (for details, see section 10).
2.2 Glossary 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 (for details, see section 7). Interface The «IC Net» program supports remote control for interfaces available from Metrohm and Bischoff.
2 Fundamentals of the operation 2.3 Overview of program windows «IC Net 2.0» consists of different windows whose functionality is linked together. The different windows are: 2.4 IC NET Main program window with menus for file administration, printing, method modification, options, login and user rights, window handling. CHROMATOGRAM Chromatogram window for graphic plot of running or recorded chromatograms. SYSTEM System window for control of interfaces and devices.
2.5 Icons of the main window 2.5 Icons of the main window The following icons are displayed in the IC NET main window: Open chromatogram Save chromatogram Open last batch reprocessing file Make report Print preview Send chromatograms to Autodatabase Print chromatogram Passport Method setup Integration Components Cascade all opened chromatogram windows Vertical tiling of open chromatogram windows Horizontal tiling of open chromatogram windows Appearance Enable/disable peak editor mode.
2 Fundamentals of the operation 2.6 Overview of file types The following file types are produced by the «IC Net» software: 10 *.adb Autodatabase file Contains chromatogram and method data of all determinations. *.bar Batch reprocessing file (binary file) Contains batch reprocessing data. The *.bar file is stored automatically in the Data folder. *.cal Calibration file (binary file) Contains calibration data, which can be exported with IC Net / Method / Calibration / Export calibration. The *.
2.7 Context-sensitive menus 2.7 *.rtt Report file (ASCII file) Contains a report template. The *.rtt file is stored in the program folder. *.smt System file (ASCII file) Contains the system settings. The *.smt file is stored automatically in the Systems folder. *.dev Device file (ASCII file) Contains drivers for devices. The *.dev file is stored in the Devices folder.
2 Fundamentals of the operation Shifts a chromatogram on 1/10 part of a screen downwards. [ Shift ] + [ up ] Increases a distance between channels of a chromatogram. [ Shift ] + [ down ] Reduces a distance between channels of a chromatogram. [ 0 (Zero) ] Adjusts a zero on the last point of a chromatogram (running chromatogram) or its lowest level (finished run). Only part of the chromatogram is on screen: [ Ctrl ] + [ right ] Moves one window right (without change of scale on X and Y axes).
3.1 Fonts 3 Software settings 3.1 Fonts IC NET / Options / Fonts This option allows the selection of fonts used by the system. Font for dialogs... 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.
3 Software settings ences, open the Workplace window, change hardware settings of interfaces and devices, and change Security options. Administrator Access to all program functions. This level should be switched on only while installing the system or in the case of configuration change. The administrator user is authorized to change access levels, names and passwords of other users It is recommended to make user lists and enter passwords as a first action after software installation.
3.3 Global settings Data file overwrite Never Ask Always If method changed Don't ask to save Ask to save Global settings for overwriting of chromatogram files: Chromatogram files cannot be overwritten. A modified chromatogram is saved as new file with the file name number raised by 1. The user is asked if the chromatogram should be overwritten. Chromatogram files are always overwritten without confirmation. Global settings for saving of method files: The method file is not saved automatically.
3 Software settings Ignore last data directory If this option is enabled, the directory is opened where the current selected chromatogram is saved. If this option is disabled, the directory is opened where the last opened chromatogram is saved. GLP On Switch on/off global GLP settings.
4.1 System creation 4 Systems The combination of Metrohm and Bischoff devices connected to an interface is called a system. The system includes all the settings of the devices, their time program, the data acquisition parameters and the 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 (*.
4 Systems , the interface icon will appear on the toolbar (PC Boards will not appear on toolbar). After clicking on , the window for addition of devices (see 6.1.1) to the system window appears. For every device to be controlled with «IC Net», open the group which contains this device, select the device and the Serial port of the interface where the device is connected to. After clicking on , the device is added to the SYSTEM window.
4.1 System creation After clicking on , the user is asked to save the new system as a system file (*.smt) in the new system folder. The new system is now ready to start a determination (see section 4.3.3). 4.1.2 System window A system window is opened with IC NET / File / Open / System and the selection of the desired system file. It contains icons for Data recorder, Watch window (screen) and all the devices installed with the system wizard. Watch window Data recorder 4.1.
4 Systems 4.2 System file handling The following menu items are used for opening, changing, saving and closing of systems: IC NET / File / Open / System Load an existing system file (*.smt) from the Systems directory and open the corresponding SYSTEM window. The name of the folder and of the system file are displayed in the title bar of the SYSTEM window. A star ( * ) at the end of the name indicates that the system settings have been changed since the last saving.
4.3 System functions SYSTEM / Control / Disconnect from workplace Disconnect selected system from the workplace. If a system is disconnected, manual control is not available for this system, but all other system settings can be modified and saved. Start determination and Startup hardware is only possible if no other system from the same system folder is connected. In this case, the system is automatically connected. 4.3.
4 Systems 4.3.3 Start/stop determinations SYSTEM / Control / Start determination Start determination using the settings of the selected system. At this start command, the System startup values are set at the devices. The time programs of the different devices and the data recording are started either immediately (Start with determination) or after switching the injection valve to the "Inject" position (Start with inject) as set in the Start mode window.
4.3 System functions Ident Calibration level Info 1 / Info 2 Volume Dilution Vial number Amount 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 (0 = sample; 1…n = calibration solutions). Sample description. Injected volume in µL. Dilution of the sample. Autosampler vial position to take sample from. Sample amount.
4 Systems 4.4 System settings 4.4.1 Modify system window SYSTEM / Setup / Drag icons If this option is enabled, the device icons can be resized and moved in the SYSTEM window and the SYSTEM window itself can be resized. To resize an icon or the window, move the cursor to the desired object until appears. Press the left mouse button and resize the object to the desired size. To move an icon, move the cursor to the desired object until appears.
4.4 System settings The time program of the loaded object or the data acquisition (RECORDER) is started at the moment the sample is injected. Start with inject The objects can be moved from one field to the other using the or 4.4.4 buttons. Install new devices SYSTEM / Setup / New devices/ Install new device Add new devices to the open SYSTEM window.
4 Systems 4.4.7 Show system parameters SYSTEM / Setup / Parameters / Startup hardware Display of the name of the method linked to the system, the main measurement channel, the configuration settings for the devices, and the system startup values. SYSTEM / Setup / Parameters / Start with determination Display of the objects defined in the Start mode window. The time programs are displayed if the programs are enabled.
4.5 System state window 4.5.2 Running Running program or chromatogram data acquisition. Running program (xxx min left) Running time program with time display. Waiting for INJECT Waiting for "INJECT" to start program and/or chromatogram data acquisition as defined in the Start mode. INJECT done Injection valve has been switched to the "INJECT" position. Stopping Determination has been stopped. Finished Program or chromatogram data acquisition has been finished. SHUTDOWN System is shutdown.
4 Systems 28 E295 Storage of memory values failed (repeat last action; if error reappears, call Metrohm service). E296 Instrument stopped (restart instrument; if error reappears, call Metrohm service). E297 Storage of remote line values failed (repeat last action; if error reappears, call Metrohm service). E298 Storage of flow correction value failed (repeat last action; if error reappears, call Metrohm service).
5.1 Interface installation 5 Interfaces The «IC Net» program supports remote control for interfaces available from Metrohm and Bischoff. Interfaces generally convert analog signals to digital form, which can be handled by the computer. Interfaces are stored as device files (*.dev) in the Devices directory. All Metrohm interfaces and Metrohm devices start with Me*.dev; all Bischoff interfaces and Bischoff devices start with Bi*.dev. 5.1 Interface installation 5.1.
5 Interfaces Details to the other steps of the system wizard procedure (installation of devices, processing method, and data source) see section 4.1.1. 5.1.2 Add interfaces in workplace window IC NET / Options / Devices setup Open the WORKPLACE window which shows all interfaces and devices installed. This window can be opened only by the user with Administrator access level. Click on to open the Adding interfaces to your workwindow and proceed as described in section 5.1.1. place 5.1.
5.2 762 IC Interface 5.2 762 IC Interface 5.2.1 762 IC Interface features The Metrohm 762 IC Interface is available as a one system version (2.762.0010) or a two system version (2.762.0020). Each system can control a complete ion chromatography or HPLC equipment and contains the following parts: • Two 24-bit Analog-to-Digital Converters (often abbreviated as ADC) to acquire two analog signals from two different detectors simultaneously (for example conductivity detection and UV detection).
5 Interfaces 5.2.4 762 IC Interface window 762 icon / Open The 762 IC Interface window for parameter settings is opened by selecting this menu option with the right mouse button or by clicking the 762 icon on the toolbar. It consists of three tabs Init, RS settings, and Links. Init The Init tab of the 762 IC Interface window contains data acquisition parameters for the 762 IC Interface. Label Optional label to name the interface with maximum 8 characters.
5.2 762 IC Interface Read current parameters from 762 IC Interface. Send current parameters to 762 IC Interface. RS settings The RS settings tab of the 762 IC Interface window contains RS232 parameters for the 762 IC Interface. Baud Rate Parity Handshake FIFO size IC Net 2.0 Baud rate of the device. Selection: 1200...115200 Default value: 115200 Parity check. Selection: None, Even, Odd Default value: None Enable/disable software handshake mode.
5 Interfaces Links The Links tab of the 762 IC Interface is used for COM port selection and settings. Alias Name of the interface or device. COM # If this entry is clicked with the right mouse button, the following menu appears: Possibility for setting COM port parameters (details see on-line help). Possibility for changing the COM port. The following window is opened, where the COM port can be changed by clicking on the desired entry. Put on desktop Change 5.2.
5.2 762 IC Interface Time program On the Program tab of the 762 System [#] window a user-defined time program for the event output lines of the 762 IC Interface can be entered. This program is started automatically as defined in the Start mode window (see section 4.4.3) either at the moment the determination is started (Start with determination) or at the moment the sample is injected (Start with inject).
5 Interfaces Add new program instruction. Delete selected program instruction. Test the time program (error messages are displayed if program is wrong). List of program instructions The following program instructions can be added to the time program on the Program subpage: Instruction Parameter entry Meaning Events 0, 1, p, * Set event output lines 1...7 to the desired values. For entry of the first value, enter 1, 0, p or *.
5.2 762 IC Interface Event command (2nd column) Setting the event output lines 1…7. Selection: 0 (line off, inactive, open) 1 (line on, active, 0 V) p (pulse, pulse length 150 ms) * (leave line in current status) For entry of the first value, enter 1, 0, p or *. For entry of the other values, move the cursor in front of the value to be changed and enter 1, 0, p or *. Add new remote command. Delete selected remote command.
5 Interfaces 5.3 771 Compact Interface 5.3.1 771 Compact Interface features The Metrohm 771 Compact Interface is a two channel Analogto-Digital Converter to acquire two analog signals from two different detectors simultaneously or time independent. It contains the following parts: • Two 24-bit Analog-to-Digital Converters (often abbreviated as ADC) to acquire two analog signals from two different detectors simultaneously (for example conductivity detection and UV detection). • Two external start inputs.
5.3 771 Compact Interface Range Range for AD converter. Example: converts ± 2500 mV to 224 bits Entry range: 2500, 1250, 625, 312.5, 156.25, 78.125, 39.062 mV Read current parameters from 771 Compact Interface. Send current parameters to 771 Compact Interface. RS settings The RS settings tab of the 771 Compact Interface window contains RS232 parameters for the 771 Compact Interface. Baudrate Parity IC Net 2.0 Baud rate of the device. Selection: 1200...
5 Interfaces Handshake Enable/disable software handshake mode. Selection: Swchar, none Default value: SWchar Read current parameters from 771 Compact Interface. Send current parameters to 771 Compact Interface. Links The Links tab of the 771 IC Interface is used for COM port selection and settings (details see section 5.2.4). 5.4 761 Compact IC 5.4.1 761 Compact IC features The Metrohm 761 Compact IC is a PC-controlled system for ion chromatographic analyses.
5.4 761 Compact IC 5.4.3 761 icon in the system window System disconnected System connected Injection valve in "INJECT" position System connected Injection valve in "FILL" position The 761 icon is available in the system window if a 761 Compact IC has been installed with the Install existing devices option (see section 6.1.3).
5 Interfaces Conductivity, µS/cm Live display of measured conductivity. Pressure, MPa Live display of measured pressure. The color settings for this two fields can be changed by clicking the fields with the right mouse button (see section 6.2.2). Display of actual values. Flow, mL/min Display of current flow rate of the highpressure pump. Pressure max, MPa Display of current maximum pressure limit for high-pressure pump.
5.4 761 Compact IC IC pump Peristaltic pump High-pressure pump. Start high-pressure pump. Stop high-pressure pump. Peristaltic pump. Start peristaltic pump. Stop peristaltic pump. The system startup values are sent and applied to the 761 Compact IC each time the system is connected, a determination is started, or the values are sent manually with . Flow, mL/min Startup value for flow rate of the highpressure pump. Entry range: 0.20 ... 2.
5 Interfaces Pressure max, MPa Pressure min, MPa Full scale, µS/cm Remote lines 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 ... 25.0 MPa Startup value for full scale range. Selection: 50, 250, 1000 µS/cm Startup value for remote line settings 1…8.
5.4 761 Compact IC Second column Program instruction (see below). In addition to these predefined instructions, user-defined remote commands can be entered if activated on the Remote configuration tab. Third column Parameter for program instruction (see below). ENABLED Enable program start (a disabled program is not started). Add new program instruction. Delete selected program instruction. Test the time program (error messages are displayed if program is wrong).
5 Interfaces Program END, RESET Switch suppressor module to the next position. Suppressor Peristaltic The END flag can be used to end a program, especially if the program time should be longer than the chromatogram duration. Additional steps after this flag are not allowed. The RESET flag is used to reset the parameters to the system startup values. Switch on or off the peristaltic pump.
5.4 761 Compact IC Configuration The Configuration tab in the system settings window contains configuration settings for the 761 Compact IC. 761 unit version Selection of instrument version: 761.0010 = 761 Compact IC without suppressor 761.0020 = 761 Compact IC with 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.
5 Interfaces 5.4.5 Hardware settings Selection of the Hardware menu item of the 761 icon using the right mouse button opens the hardware settings window consisting of the three tabs Hardware, Outputs and Alarm stops. Hardware The Hardware tab of the hardware settings window defines general parameters which are set automatically at power on of the 761 Compact IC. Remote lines after power on The remote output lines 1…8 are set to this values after power on or a manual stop with Shutdown hardware.
5.4 761 Compact IC 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. Range: 0.1 ... 1000 /cm For a precise determination of the cell constant, pump a calibration solution of known conductivity through the IC system, observe the displayed conductivity and change the cell constant until the correct conductivity value is displayed.
5 Interfaces Hardware error detected at the 761 Compact IC (high-pressure pump, injection valve, or suppressor not working correctly). Alarm leak detector Leak detector has detected solvent in the instruments interior. Hardware error Remote line Set remote output lines 1…8. Selection: 0 (line off, inactive, open) 1 (line on, active, 0 V) p (pulse output) * (leave line in current status) PowerOn values Display of the power on startup values for remote output lines set on the Hardware tab.
5.5 Metrohm PC Board 5.5 Metrohm PC Board The 2.714.0310 Metrohm PC Board Interface is a two channel Analog-to-Digital Converter (often abbreviated as ADC) to acquire two analog signals from two different detectors simultaneously or time independent (e.g. conductivity detection and UV detection). One or two PC Boards can be installed in the same PC: PC Board 1 is the first interface, PC Board 2 is the second interface installed in the PC. They differ in different jumper settings on the board.
5 Interfaces 5.6.2 Timer program The Timer window contains the user-defined program for system tasks. These tasks are started automatically at the day and time defined in the program. The title line of the Timer window shows the current time left in days:hours:minutes:seconds until the next task is automatically started. Add a new task to the timer program. Selecting this option opens a subwindow for selection of the days at which the task should be started.
6.1 Device installation 6 Devices The «IC Net» program supports remote control for Metrohm and Bischoff instruments. Each instrument within a system is a device. Devices are stored as device files (*.dev) in the Devices directory. All Metrohm devices start with Me*.dev and all Bischoff devices start with Bi*.dev. 6.1 Device installation 6.1.1 Install devices at system creation IC NET / File / New / System The New system wizard window and a new SYSTEM opened.
6 Devices For every device to be controlled with «IC Net», open the group which contains this device, select the device and the Serial port of the interface where the device is connected to. After clicking on , the device is added to the SYSTEM window. If desired, an additional data recorder and a timer of the More modules group can be added to the system. Details to the other steps of the system wizard procedure (processing method, data source) see section 4.1.1. 6.1.
6.2 Watch window 6.2 Watch window 6.2.1 Watch window icon The watch window icon is one of the components always present in a new SYSTEM window. If the system is connected and this icon is clicked with the right mouse button, the following menu item appears: 6.2.2 Open Open the WATCH WINDOW for live display of instrument values (this window can also be opened by double-clicking the watch window icon). Unlink Delete the WATCH WINDOW from the SYSTEM window (not recommended).
6 Devices The colors of the watch window fields and of the SYSTEM STATE window can be changed by clicking the fields with the right mouse button. This offers the following possibilities: Choose color / Foreground / Out of range Set display color for field numbers if the measurement value is out of range (overflow or out of limits). Choose color / Foreground / In range Set display color for field numbers if the measurement value is inside the normal range.
6.3 732 IC Detector 6.3 732 IC Detector 6.3.1 732 IC Detector features The Metrohm 732 IC Detector is a conductivity detector for ion chromatography. The associated thermostatable detector block can be used for recording of chromatograms with and without chemical suppression and is normally installed in the 733 IC Separation Center. The two following versions are available: • 2.732.0010 IC Detector with standard detector block • 2.732.
6 Devices 6.3.3 732 IC Detector window 732 icon / Open The 732 IC Detector window for parameter settings is opened by selecting this menu option with the right mouse button or by double-clicking the 732 icon in the SYSTEM window. It consists of the four tabs Display, Method parameter, Program, and Links. Display The Display tab of the 732 IC Detector window is only available for a connected system. It displays the current measurement values and parameters settings of the 732 IC Detector.
6.3 732 IC Detector Range Full scale Cell const. Thermostat Offset Damping Display of measuring range in µS/cm. Display of full scale range in µS/cm. Display of cell constant of the conductivity cell in /cm. Display of temperature within in the detector block. Display of offset of the zero point. Display of electronic damping of the analog output. Zero Triggers the auto-zero function. Switch off the auto-zero function. Update all display values.
6 Devices Range Measuring range in µS/cm Selection: 100, 200, 500 µS/cm and 1, 2, 5, 10 mS/cm Full scale The full scale range (operating range) sets the desired sensitivity for the analog output. The possible values of the full scale range in µS/cm depend on the preset measuring Range. Ion Combination of polarity and temperature coefficient: Anion polarity = +, temperature coeff. = 2.5 Cation polarity = –, temperature coeff. = 1.5 Custom independent selection of polarity and temperature coeff.
6.3 732 IC Detector The Program tab contains the two following subpages: Program Remote configuration Main time program with all program steps. Possibility for creation of user-defined remote commands. Program On the Program subpage, program steps including time, program instruction and parameter can be entered. First column Second column Third column ENABLED Will be executed by IC Net 2.0 Time at which program instruction is applied. Entry range: 0.0 ... 999.
6 Devices List of program instructions The following program instructions can be added to the time program on the Program subpage: Instruction Parameter entry Meaning Remote 0, 1, * Set remote output lines 1...8 to the desired values. For entry of the first value, enter 1, 0 or *. For entry of the other values, move the cursor in front of the value to be changed and enter 1, 0 or *. Flag reset, end Set program flag.
6.3 732 IC Detector Pmax 0.0 ... 25.0 MPa Set maximum pressure limit for the high-pressure pump connected to the 732 IC Detector to the desired value. Pmin 0.0 ... 25.0 MPa Set minimum pressure limit for the high-pressure pump connected to the 732 IC Detector to the desired value. Remote configuration On the Remote configuration subtab user-defined remote commands can be defined, which can be inserted into a time program after being activated with .
6 Devices 6.4 733 IC Separation Center 6.4.1 733 IC Separation Center features The Metrohm 733 IC Separation Center is a thermally and electronically isolated wet part which accommodates injectors, columns, detectors, suppressor module and pulsation dampener and is controlled by and connected to the 732 IC Detector. The following versions are available: • • • • 2.733.0010 IC Separation Center with 1 injector 2.733.0020 IC Separation Center with 2 injectors 2.733.
6.4 733 IC Separation Center If the system is connected and the 733 icon is clicked with the right mouse button, the following menu appears: 6.4.3 Open Open the 733 IC Separation Center window for parameter settings (this window can also be opened by double-clicking the icon). Unlink Delete the 733 icon from the system.
6 Devices Suppressor in position Display of current suppressor status. Switch suppressor module to next position. Auto Step fill, inject, off Entry field Display of current auto step status. Set automatic switching of the suppressor module after each "fill" or "inject" of valve A. Selection: fill, inject, off Links The Links tab of the 733 IC Separation Center is used for COM port selection and settings (details see section 5.2.4). 6.5 709 IC Pump 6.5.
6.5 709 IC Pump 6.5.2 709 IC Pump icon The 709 icon is available in the SYSTEM window if an Isocratic pump 709 or an Isocratic pump 709 for 732 has been installed with the New system wizard or by using the Setup/New devices/Install new device option of the SYSTEM window (see section 6.1.2). If the system is connected and the 709 icon is clicked with the right mouse button, the following menu appears: 6.5.
6 Devices Pressure Flow Live display of current pressure in MPa. This field is also available for the WATCH WINDOW. Live display of current flow in mL/min. This field is also available for the WATCH WINDOW. New flow A new flow can be set by moving the scroll bar, by entering a value or by changing the value using the up and down arrows. Entry range: 0.01 ... 5.00 mL/min Min/Max pressure The minimum and maximum pressure limit for the 709 IC Pump can be set in steps of 0.1 MPa. Entry range: 0.0 ... 50.
6.6 Metrohm solvent delivery unit Advanced The Advanced tab of the 709 IC Pump window is only available for a connected system. Correction factor Flow correction factor to adjust the displayed flow to the actual flow measured with the aid of a measuring cylinder. Entry range: 0.90 ... 1.10 Read current Correction factor value. Send current Correction factor value to the 709 IC Pump. This parameter is not stored in the system file (*.smt) as long as the file is not saved. 6.
6 Devices 6.6.2 Metrohm SDU icon The SDU icon is available in the SYSTEM window if an SDU (Solvent Delivery Unit) has been installed with the New system wizard or by using the Setup/New devices/Install new device option of the SYSTEM window (see section 6.1.2). The SDU icon consists of one to four 709 IC Pump icons one above the other depending on the SDU type installed. If the system is connected and the SDU icon is clicked with the right mouse button, the following menu appears: 6.6.
6.6 Metrohm solvent delivery unit Pressure Flow New flow A new flow can be set by moving the scroll bar, by entering a value or by changing the value using the up and down arrows. Entry range: 0.01 ... 20.00 mL/min (depending on number of pumps) Min/Max pressure The minimum and maximum pressure limit for the individual pump units can be set in steps of 0.1 MPa. Entry range: 0.0 ... 50.0 MPa. %B Individual flow rate for pump B in percent of total flow. Entry range: 0 ...
6 Devices Program The Program tab of the SDU window contains a time program for the pump control system to define eluent gradients. Flow Overall flow of pump control system in mL/min. This value is also available for the WATCH WINDOW. This field is only available if the Show flow column option is disabled. Entry range: 0.01 ... 20.00 mL/min (depending on number of pumps) Stop pumps after the run Stop pumps after the determination.
6.6 Metrohm solvent delivery unit %D Individual flow rate for pump D in percent of total flow. Entry range: 0 ... 100 % Enabled Enable time program start (a disabled program is not started). Show flow column Show Flow column in the program table. Add a new line to the time program. Delete the selected line from the time program. Start all pump drives. Interfaces The Interfaces tab of the SDU window is only available for a connected system.
6 Devices 6.7 752 Pump Unit 6.7.1 752 Pump Unit features The Metrohm 752 Pump Unit is a 2-channel peristaltic pump which is normally used for operating the suppressor module in the 733 IC Separation Center by supplying regeneration and rinsing solutions. The 752 Pump Unit, which is normally operated manually using the keypad of the instrument or automatically via 732 IC Detector via remote interface, can be fully operated using the «IC Net» program.
6.7 752 Pump Unit Manual The Manual tab of the 752 Pump Unit window for manual operation is only available for a connected system. Pump Start pump drive. Stop pump drive. Start pump with startup hardware Automatic start of pump drive with Startup hardware. Time program On the Program tab of the 752 Pump Unit window a user-defined time program can be entered. This program is started automatically as defined in the Start mode window (see section 4.4.
6 Devices Second column Third column Program instruction (see below). Parameter for program instruction (see below). ENABLED Enable program start (a disabled program is not started). Add new program instruction. Delete selected program instruction. Test the time program (error messages are displayed if program is wrong).
6.8 753 Suppressor Module 6.8 753 Suppressor Module 6.8.1 753 Suppressor Module features The Metrohm 753 Suppressor Module consists of a control unit with a 2-channel peristaltic pump and a block containing a suppressor module. The 753 Suppressor Module, which is normally operated manually using the keypad of the instrument or automatically via 732 IC Detector via remote interface, can be fully operated using the «IC Net» program.
6 Devices Manual The Manual tab of the 753 Suppressor Module window for manual operation is only available for a connected system. Pump Start pump drive. Stop pump drive. Suppressor Rotate suppressor to the next position. The time since the last step action is displayed in the field beside the button. Start pump with startup hardware Automatic start of pump drive with Startup hardware.
6.8 753 Suppressor Module First column Second column Third 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. Program instruction (see below). Parameter for program instruction (see below). ENABLED Enable program start (a disabled program is not started). Add new program instruction. Delete selected program instruction.
6 Devices 6.9 754 Dialysis Unit 6.9.1 754 Dialysis Unit features The Metrohm 754 Dialysis Unit is a unit for on-line sample dialysis before sample injection. It consists of a 2-channel peristaltic pump and a dialysis cell. The 754 Dialysis Unit, which is normally operated manually using the keypad of the instrument or automatically via 732 IC Detector via remote interface, can be fully operated using the «IC Net» program.
6.9 754 Dialysis Unit Manual The Manual tab of the 754 Dialysis Unit window for manual operation is only available for a connected system. Pump Start pump drive. Stop pump drive. Start pump with startup hardware Automatic start of pump drive with Startup hardware. Time program On the Program tab of the 754 Dialysis Unit window a user-defined time program can be entered. This program is started automatically as defined in the Start mode window (see section 4.4.
6 Devices Second column Third column Program instruction (see below). Parameter for program instruction (see below). ENABLED Enable program start (a disabled program is not started). Add new program instruction. Delete selected program instruction. Test the time program (error messages are displayed if program is wrong).
6.10 750 Autosampler 6.10 750 Autosampler 6.10.1 750 Autosampler features The Metrohm 750 Autosampler is a sampler for automatic sample injection for ion chromatography. It has a capacity of up to 128 samples each with an effective volume of ca. 700 µL. The 750 Autosampler, which is normally operated using the keypad of the instrument, can be fully operated using the «IC Net» program. The 750 Autosampler is normally connected to the 762 IC Interface using the 6.2134.
6 Devices 6.10.3 750 Autosampler window 750 icon / Open The 750 Autosampler window for parameter settings is opened by selecting this menu option with the right mouse button or by double-clicking the 750 icon in the SYSTEM window. It consists of the four tabs Manual, Injection, Diagnostics and Links. Manual The Manual tab of the 750 Autosampler window for manual operation is only available for a connected system.
6.10 750 Autosampler Loop size is Size of the sample loop at the 733 IC Separation Center. If the loop size is > 20 µL, only 3 injections per sample vial are possible. Move transfer needle to the desired vial position (1...128 or Home). Lower transfer needle to the desired position (1...4). Start manual rinsing using the desired vial (1...128).
6 Devices Manual injection Sample vial number
6.11 766 IC Sample Processor 6.11 766 IC Sample Processor 6.11.1 766 IC Sample Processor features The Metrohm 766 IC Sample Processor is a sampler for automatic sample injection for ion chromatography. It has a capacity of up to 127 samples each with an effective volume of up to 11 mL. The 766 IC Sample Processor, which is normally operated using the keypad of the instrument, can be fully operated using the «IC Net» program.
6 Devices If the system is connected and the 766 icon is clicked with the right mouse button, the following menu appears: 6.11.3 Open Open the 766 IC Sample Processor window for parameter settings (this window can also be opened by double-clicking the icon). Unlink Delete the 766 icon from the system.
6.11 766 IC Sample Processor Position Selection of the vessel to be placed at the needle. Selection: sample, sample+1, spec.#, 1...n Lift Position Start raising or lowering the lift to the specified position. Stop raising or lowering the lift to the specified position. Selection of the position. Selection: shift, work, rinse, special, 0, 1...125 mm Pump Time Switch on peristaltic pump at the tower for the specified time. Switch off peristaltic pump at the tower.
6 Devices Status display The current status of the 766 IC Sample Processor can be displayed on the Current state subtab of the Manual tab which is only available for a connected system. Sample Beaker position Lift position Pump state Display of current sample position. Display of current beaker position. Display of current lift position in mm. Display of current pump state (on, off). Status of the 8 input lines Status of the remote input lines.
6.11 766 IC Sample Processor Num Task Parameter Row number (read-only). Program instruction (see below). Parameter for program instruction (see below). Enabled Enable program start (a disabled program is not started). Add new program instruction. Delete selected program instruction. List of program instructions The following program instructions can be added to the time program on the Program tab: IC Net 2.0 Instruction Parameter entry Meaning Move sample, sample+1, spec.#, 1...
6 Devices Ctrl "control command" Set the specified remote output signal. In addition to the normal control commands (details see 766 Instruction for Use) special commands defined on the Configuration tab can be used. Wait 1...9999 s Waiting time. StartDA Start data acquisition. Configuration The Configuration tab of the 766 IC Sample Processor window contains parameters settings on the five subtabs Rack, Beaker positions, Needle positions, Control, and Scan.
6.11 766 IC Sample Processor Beaker positions Rack type Current rack type (read-only). Parameter Name for special beaker position. Number of special beaker position. Pattern Add a new special beaker position. Delete the selected special beaker position. Needle positions Rack type Current rack type (read-only). Parameter Name for special needle position. Lift position of special needle position in mm. Pattern IC Net 2.0 Add a new special needle position.
6 Devices Control Pattern Name for special control command. Remote line settings for special control command. Add a new special control command. Delete the selected special control command. Parameter 94 IC Net 2.
6.11 766 IC Sample Processor Scan Pattern Name for special scan command. Remote line settings for special scan command. Add a new special scan command. Delete the selected special scan command. Parameter Links The Links tab of the 766 IC Sample Processor is used for COM port selection and settings (details see section 5.2.4). IC Net 2.
6 Devices 6.12 Data recorder 6.12.1 Data recorder icon The Data recorder icon is one of the components always present in a new SYSTEM window. If the system is connected and this icon is clicked with the right mouse button, the following menu appears: Open Load the processing method linked to the system and open an empty chromatogram window (this window can also be opened by doubleclicking the icon). Setup Open data recorder setup window for selection of processing method and data source (see below.
6.12 Data recorder Processing method Connected data source Name of the method file (*.mtw) linked to the system. Open processing method. Select the method file (*.mtw) to be linked to the system. Data source for main measurement channel. Open the Data source window for selection of the data source: Connected data source. Connected Available 762 IC Interface # ch1 to ch4 Data source channels of the 762 IC Interface.
6 Devices 6.13 System timer 6.13.1 Timer icon The system timer is used for programming system tasks which are started automatically daily or once at the desired time. The System timer icon is available in the SYSTEM window if a Timer has been installed with the New system wizard or by using the Setup/New devices/Install new device option of the SYSTEM window (see section 6.1.2). 6.13.2 Timer program The timer program of the system program is identical to the global timer program (see section 5.6.2).
7.1 Method file handling 7 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. Each system is linked to a method. This method is called processing method and is opened automatically at the start of a new determination. 7.
7 Methods 7.2.1 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 100 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 min. You can modify this value when the chromatogram is running.
7.2 Passport Run Number of the current run starting from the very first one. All runs are automatically numbered by the system (read-only). 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 7.2.2 Sample Tab Sample of the passport with sample information. Info 1 Info 2 Volume Dilution Vial number Amount IC Net 2.
7 Methods Internal standard amount Concentration of the internal standard component for relative concentration calculations. Date/time when... 7.2.3 Column Date and time of sample collection (the default values are equal to the date and time when the chromatogram starts). 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.
7.2 Passport 7.2.4 Eluent Tab Eluent of passport with eluent information. Eluent A Eluent B Eluent C Flow Pressure Temp. IC Net 2.0 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 or µL/min. The flow rate is used to recalculate the time axis into volumetric units.
7 Methods 104 7.2.5 Comment 7.2.6 Method Log Tab Comment of passport for entry of free-text user comments into the chromatogram description. Use this feature to enter any additional information about the chromatogram not included in other sections of the method. 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 this messages free-text user comments can be entered.
7.2 Passport 7.2.7 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 this 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. IC Net 2.0 Add a new GLP comment to the Method Log.
7 Methods 7.3 Method setup IC NET / Method / Method setup This menu item opens the Method setup window which includes the most common parameters for data acquisition and evaluation of the method and consists of the following tabs: General Measure Filters Processing Math 7.3.1 General 7.3.2 Measure General information on determination. Important data acquisition parameters. Parameters for noise filtration. Set actions that are performed when the chromatogram finishes.
7.3 Method setup 7.3.3 Filters Tab Filters of Method setup window with parameters for noise filtration of raw data. Three different filtration algorithms are available to reduce noise and increase apparent signal-to-noise ratio. Spikes Slit Median Slit Gaussian Raw data points Smallest peak has ... IC Net 2.0 Spikes filter. The Spikes filter smoothes the first and last points of the chromatogram and the points identified as spikes.
7 Methods 7.3.4 Processing Tab Processing of Method setup window for definition of actions that are performed during the run or when the chromatogram finishes. Automatic post-run data processing is especially useful for chromatographic systems that include an autosampler. Save chromatogram after the run If checked, autosaving of the chromatogram will be performed on data acquisition ending. while running every ...
7.3 Method setup Program before Program after 7.3.5 Math Tab Math of Method setup window with parameters that are used for various types of calculations. Parameter Formula set Theoretical plates Resolution Asymmetry Formula Custom formulae IC Net 2.0 Name and path of the program to be started automatically before the run is started. Name and path of the program to be started automatically after the run is finished.
7 Methods European Pharmacopoeia Formula setting according to European Pharmacopoeia. US Pharmacopoeia Formula setting according to US Pharmacopoeia. Calculation of void time/void volume: Calculation method Selection of the method for void time calculation: None Manual entry in the Void time field. 1st component 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.
7.4 Integration 7.4 Integration 7.4.1 General information IC NET / Method / Integration This menu item opens the Integration parameters window which contains parameters and events for peak integration and consists of the two tabs Setup (see section 7.4.2) and Events (see section 7.4.3). The «IC Net» software includes a built-in automatic integration algorithm to detect peaks on the chromatographic curve and to evaluate them using calculated baselines.
7 Methods 7.4.2 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).
7.4 Integration Broadening Slope Asymmetry Min area Min height Rider ratio Negative peaks width of the narrowest peak on the chromatogram (normally 2…10 s). Entry range: 0.1… …480 s Broadening for peaks in the end of the chromatogram compared to peaks in the beginning. This parameter is used for automatic adjustment of Width. Entry range: 0.1… …100 Threshold for peak recognition.
7 Methods 7.4.3 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. Number of events Number of integration events (read-only). Add event to the list. Edit the selected event.
7.4 Integration If an integration event is added or modified, the Edit integration event window is opened where the following parameters can be set: Time Event Value Start time for integration event in min. List box with integration events to be selected (see below). Parameter value for selected integration event. This field appears for events that demand input of an additional parameter. Integration events for peak detection Set this mode to stop detection of new peaks.
7 Methods Integration events for peak start/end Force the beginning of a new peak. If a peak is available at the moment of the event it is either rejected (upslope) or terminated (downslope). Set peak end Force peak end at the time of the event. Upslope peaks are rejected (except those born by Set peak start event), downslope peaks are terminated. Stop single peak mode Disable peak end detection. All peaks of any group after this event will be treated as one peak. The group end will be treated as peak end.
7.4 Integration Set horizontal baseline Set horizontal baseline for all peaks except the last one of adjacent peaks that are not separated. The baseline is drawn forwards from the peak start point. Set back horizontal base Set normal baseline Set horizontal baseline for all peaks except the first one of adjacent peaks that are not separated. The baseline is drawn backwards from the peak end point. Set default baseline detection mode. Set baseline point at 4.5, 6, 7.2, 8.9 and 9.
7 Methods Force horizontal base back Cancel horizontal base back Force horizontal base back Set horizontal baseline for a single peak. The baseline is drawn backwards from the peak end point. The intersection of the baseline with the signal is defined as peak start point. Cancel horizontal base back Clear Force horizontal base back mode. Enable baseline penetration Disable baseline penetration Enable baseline penetration Allow crossing of the signal by the baseline.
7.5 Calibration and quantification 7.5 Calibration and quantification 7.5.1 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.
7 Methods 7.5.2 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 C Concentration of the component in the initial solution (before dilution). Q = C • V' Quantity t Retention time. t0 Void time. t' = t – t0 Corrected retention time, L Column length. v = L / t0 Linear Flow rate.
7.5 Calibration and quantification 7.5.3 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.
7 Methods 122 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.
7.5 Calibration and quantification min C (max C) Minimum (Maximum) concentration value for the component. Components whose concentration leaves the range min C… …max C are marked in the peak table by the sign " ! ". Additionally, the component 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 section 7.5.5).
7 Methods 7.5.5 Peak identification IC NET / Method / Calibration / Identification Selecting this menu item or clicking on in the component table opens the Peak identification window with parameters for tuning the peak identification procedure. Number of components Number of components in the component table (read-only). Scheme Standard Nonstandard Identification Reference peaks Other peaks Identification parameters. Identification parameter for reference components.
7.5 Calibration and quantification Worst case... Information on the component with the worst (largest) deviation of actual and expected retention time. Deviation is given as a part of component’s identification window. Average relative deviation Relative deviation averaged for all components. 7.5.
7 Methods Level 1...Level N Contains concentrations (or other chosen values) of components for corresponding Calibration level. 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.
7.5 Calibration and quantification 7.5.7 Calibration curve IC NET / 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.
7 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.
7.5 Calibration and quantification 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 Formula for calibration function. There are six possible calibration dependencies for linear and nonlinear calibration curves.
7 Methods Coef. (balance) 7.5.9 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. Calibration data handling Load and save calibration data IC NET / Method / Calibration / Load from method Load the calibration from the method.
7.6 Report output 7.6 Report output 7.6.1 Report options window IC NET / Method / Report options IC NET / 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 . IC Net 2.
7 Methods 7.6.2 Items to report This part of the Report options window contains a list of important report items that can be included into the report on the user's choice: General Report date: Printed by: General description on the analysis from the Passport. The Report date and the logged-in user Printed by are also put out. 07/12/1999 15:59:10 Roland Dörig Ident: Tap water Analysis from: 10/11/1999 16:17:02 File: jb101617.chw 16/11/1999 15:02:14 Modified! Method: Multicalibration.
7.6 Report output Chromatogram plot Plot of the chromatogram (only for Printer or File destination). Peak table Peak table with results. The structure of the peak table depends on the selected Quantification method. The following report is put out as default: Quantitation method: Custom No Retention Height Area Conc. min mV mV*sec mg/L 1 3.04 1.85 21.062 0.079 2 5.91 82.44 1703.350 7.173 3 6.83 3.58 97.495 0.000 4 14.29 29.27 969.705 7.561 5 21.21 19.34 935.179 5.
7 Methods DATA GLP LOG Analysing data of channel :ch1 Time constant, ms: 100.00; old 100.01 Iterations: 2; Outliers: 1 Sigma: 0.0 Rejection difference: 1.0 Time error position 5, ratio 2.000, 1 missing points: CORRECTED Corrections 1, Unrecovered errors 0 10/11/1999 16:42:04 Metrohm Status: Processing Data saved to disk file c:\progra~1\metrohm\icnet2~1.0\icnet~1\data\JB101617.CHW 7.6.
7.6 Report output Calibration defaults Calibration parameters defined in the component window and on the Math tab of the Method setup window. CALIBRATION Channel: Method: Response: Standard: IDENTIFICATION Reference peaks: Other peaks: Retention units: Component table No Retention Window% 1 2 3 4 5 6 7 3.05 5.92 8.70 11.19 14.60 16.80 21.26 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Height Time min Component table. RF Conc. 2.623e-03 4.356e-03 6.691e-03 9.933e-03 7.912e-03 1.556e-02 6.021e-03 0.08 7.17 0.00 0.
7 Methods Parameters of the data acquisition channel used. Channel table CHANNELS TABLE ch1 No Name 1 ch1 # 1 Name/Units ch1 mV Units Input mV Minimum Zero 1 -8388607 0 Noise 4.2 0.00124 RMS 29976.5 8.93 Units Input Minimum Zero Maximum Range Coefficient Noise Shift (multi)Channel ratio Range Coefficient 8388607 2.500e+03 PeakToPeak 330509.6 98.5 Name 136 Maximum 2.980e-04 Noise Shift 4.15 0 Drift/hour 3585.801 1.07 Channel’s name.
7.6 Report output 7.6.4 Report destination The following output devices can be selected simultaneously in any combination as targets for report output: Screen Printer File 7.6.5 Output report (without curves) to screen. Output report to printer. Output report to file (see section 7.6.7).
7 Methods As long as no universal component is defined, only peaks with non-zero concentrations are listed. The peak table includes the following columns: Peak number, Retention time, Height, Area, Response factor, Concentration, Concentration%, Name Relative concentration Index Column test Custom Standard component 138 This quantification method uses the internal standard method to calculate the relative concentrations of the components.
7.6 Report output Concentration of std Concentration of the internal standard component for relative concentration calculations. This value is stored in This run column of the concentration table. Total % for normalization A value to which the sum of concentrations is normalized. It is used for Response normalization and Normalized concentrations quantification methods. The default value is 100. Printing order By peaks By components IC Net 2.0 Determines the order of the components in the peak table.
7 Methods 7.6.6 Template options For report output using a report template the following parameters can be modified: 7.6.7 Template Selection of the report template file *.rtt. Several templates for different languages and applications are available. Separator Defines which character separates report columns in tables. A separator other than Space is useful when the report is printed to a file and this file is imported into a spreadsheet software. Tab size Sets tab stop value for the screen window.
7.6 Report output 7.6.8 Report elements If Quantification method = Custom has been selected, the peak table can be customized on the user's choice. After clicking the button, the following columns can be included in the peak table. number Peak number. retention time Retention time of the component (in minutes, irrespective of the chosen retention units on the chromatogram graph axes). The total value in the column is equal to the chromatogram duration.
7 Methods 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..., ti = retention time, Hi = height, Ai = area of the peak. The more commonly used formula is: Ni = 5.54 (ti / wi)2, where wi is the width on the half-height of the peak.
7.6 Report output 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) / ä 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.
7 Methods type The types of components are designated by a one-letter code: 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.
8.1 Chromatogram window 8 Chromatograms 8.1 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.
8 Chromatograms During active data acquisition the elapsed time, the duration of the chromatogram or program and the current X and Y values are shown in the second field of the status bar. If the peak editor is switched on then the position of the cursor will be shown. A chromatogram can be scaled with the help of keyboard or mouse functions or through the Chromatogram axes window opened with IC NET / View / Appearance / Chromatogram axes.
8.2 Chromatogram file handling Filename Selected Directory Filename (common wildcards as * and ? are possible). Number of selected chromatograms and their total size. Path name of the working directory File window Box with the list of files residing in the working directory sorted by time (the last recorded chromatogram is at the top of the list). As additional short information on the chromatogram the two parameters Ident and Method are also displayed.
8 Chromatograms 8.2.2 Save chromatogram IC NET / File / Save / Chromatogram Save the selected chromatogram in a chromatogram file (*.chw) in the working directory. If this chromatogram has been already stored in this directory, the message File ... exists. Overwrite? appears. If it is preferable to overwrite the previous copy (for example, after the reprocessing), press the button. Pressing saves the chromatogram into the new file (a new copy of the chromatogram is created). 8.2.
8.2 Chromatogram file handling Output of raw data: Default units (float) Y values are exported in default units for the channel. Represent raw data as ADC response (integer) Y values are exported in bits. Include retention time In seconds (float) As point number 8.2.6 X values are exported in seconds. X values are exported as point number. Import chromatogram IC NET / File / Import / Chromatogram Import chromatogram of the following formats: *.
8 Chromatograms 8.3 Graphical representation 8.3.1 Appearance IC NET / 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.
8.3 Graphical representation 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.
8 Chromatograms Component name Name of the component. Component name + Quantity Name and quantity of the component. Channel labels At start In corner Label for data acquisition channel. Channel label is shown at the start of the chromatogram. Channel label is shown in the upper right corner of the chromatogram. 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.
8.3 Graphical representation 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 Line width Line width for the selected element (Axes or Channel 1...8) in % of selected plot font height. Range: 0 ... 232 Set all Set colors of all opened chromatograms automatically to the settings in the selected chromatogram window.
8 Chromatograms 8.3.2 Other graphical functions IC NET / 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. IC NET / 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.
8.4 Peak editor 8.4 Peak editor 8.4.1 Switching on/off the peak editor IC NET / Process / Peak editor The peak editor mode is used for subsequent manual correction of the automatic integration for chromatogram peaks (see section 7.4). 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.
8 Chromatograms IC NET / Peak / Select end point Move the cursor to the end of the nearest peak and select the peak. IC NET / Peak / Select valley point Move the cursor to the valley of the two nearest peaks. IC NET / Peak / Unselect peak Delete the selection. [–] Move a selected point (start, top, end, valley) to the cursor position. IC NET / Peak / Move selected point [+] Merge two neighboring peaks into a single peak.
8.5 Printing 8.5 Printing 8.5.1 Page layout for printing IC NET / 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 Selection of length units. Inches. Centimeters. Selection of page margins. Left margin. Right margin. Top margin. Bottom margin.
8 Chromatograms 8.5.2 Printer settings IC NET / File / Printer setup By selecting this menu item the Print setup window is opened where printer, paper size and format can be defined. 8.5.3 Print preview IC NET / 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. 8.5.
8.6 Miscellaneous functions 8.6 Miscellaneous functions 8.6.1 Reintegration IC NET / Process / Reintegrate This menu item opens the Integration parameters window where the reintegration of the chromatogram can be started (details see section 7.4). 8.6.2 Recalibration IC NET / Process / Calibrate This menu item opens the Recalibration window for entry of the calibration level and recalibration of the chromatogram using this level (details see section 7.5). 8.6.
8 Chromatograms 8.6.4 Data compression IC NET / Process / More / Compress Selection of this menu item opens the Raw data compression window for compression of the raw data of the active chromatogram by summing up several neighboring points. Divisor 8.6.5 Coefficient of compression (the number of data points is reduced by this value). The default value of the compression coefficient is calculated so that the width at half-height of the narrowest peak will be digitized by at least 30 points.
8.6 Miscellaneous functions 8.6.6 Autodatabase IC NET / Method / Autodatabase The Autodatabase options window contains parameters and settings for sending chromatograms to the Autodatabase program. Database file Definition of the database file (*.adb) to which chromatograms are sent manually with or automatically if the Send data to Autodatabase file option is enabled in the Processing tab of the Method setup window. Use to select a new database file.
8 Chromatograms 162 IC Net 2.
9.1 Sample queue file handling 9 Sample queue A sample queue is a table containing sample-specific data which is used to facilitate work with autosamplers and multiple analyses. The number of rows of the sample queue table defines the number of determinations which are run automatically. Once the queue has been started, the sample-specific data are transferred line-by-line to the running determination overwriting the corresponding fields of the method. A sample queue is stored in a sample queue file *.
9 Sample queue 9.2 Sample queue control 9.2.1 Sample queue overview table IC NET / File / Open / Sample queue SYSTEM / System / Sample queue These two menu items open the OPEN window for opening an existing sample queue file *.que or creation of a new sample queue file *.que by entering a new name. After confirmation with the sample queue overview table is opened showing the current status of the sample queue: No System Ident Vial Inj-s Started Level Volume 164 Row number.
9.2 Sample queue control Amount Sample amount. If this value is different for the calibration run (c) and the sample run (s), the component concentrations of the sample are calculated as follows: Cs = Cc • Amounts / Amountc Shut down system after the queue finishes If this option is enabled, the system hardware is shut down after the sample queue has been finished (all pumps are switched off), but it remains connected. 9.2.
9 Sample queue 9.2.4 Cancel last run SAMPLE QUEUE OVERVIEW / Control / Cancel last run Cancel the last run (set Started = 0 for this row). If the queue is restarted, this row is executed again. This function is only available if the sample queue has been interrupted by pressing the button. 9.2.5 Reset sample queue SAMPLE QUEUE OVERVIEW / Control / Reset Reset sample queue table (set Started = 0 for all rows).
9.3 Sample queue editor Vial Volume Dilution Amount Autosampler vial position to take sample from. Injected volume of sample in µL. Sample dilution prior to injection. Sample amount. If this value is different for the calibration run (c) and the sample run (s), the component concentrations of the sample are calculated as follows: Cs = Cc • Amounts / Amountc Internal standard amount Level Injections Done Sample Info 1 Sample Info 2 9.3.
9 Sample queue QUEUE EDITOR / Edit / Paste row(s) Paste the rows from the clipboard into the sample queue table. QUEUE EDITOR / Edit / Delete row(s) Delete the selected rows from the sample queue table. QUEUE EDITOR / Edit / Duplicate row(s) Duplicate the selected rows of the sample queue table. QUEUE EDITOR / Edit / Increment Fill selected column fields with values automatically incremented by 1. The last character of the first selected field must be a number.
10.1 Batch reprocessing queue file handling 10 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. 10.
10 Batch reprocessing 10.1.3 Save batch reprocessing queue QUEUE EDITOR / File / Save Save the batch reprocessing queue in a batch reprocessing queue file (*.bar) in the working directory. The batch reprocessing queue editor window remains open. QUEUE EDITOR / File / Save & exit Save the batch reprocessing queue in a batch reprocessing queue file (*.bar) in the working directory and close the batch reprocessing editor window. 10.2 Perform batch reprocessing 10.2.
10.2 Perform batch reprocessing Use method from file for reprocessing Selection of the desired chromatogram file whose method should be used for reprocessing. If the reprocessing includes reintegration and/or recalibration, only chromatograms recorded with the same method should be loaded into the batch reprocessing queue. Open the chromatogram selected above in the Use method... field. Open all chromatograms of the batch reprocessing queue.
10 Batch reprocessing bration parameters (component table, concentration table and calibration curve) are applied to all sample runs. Apply final calibration to all reprocessed files Apply the updated calibration to all calibration and sample runs. If this option is switched off, the calibration stored in the first chromatogram is used for all other chromatograms.
10.2 Perform batch reprocessing Modify chromatogram appearance If this option is enabled, the chromatogram Appearance parameters which have been changed after clicking the button are applied to all chromatograms. Make report Open the Appearance window for modification of the settings for chromatogram axes, labels and colors. Print report for all chromatograms using the current report settings of the selected chromatogram in the Use method... field.
10 Batch reprocessing 10.2.2 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 ] + [ ↑ ] and decreased by pressing [ Shift ] + [ ↓ ]. The chromatogram axes, labels and colors can be set in the Apwindow.
10.3 Batch reprocessing queue editor 10.3 Batch reprocessing queue editor 10.3.1 Open batch reprocessing queue editor window REPROCESS / This menu item opens the batch reprocessing editor program for editing the batch reprocessing table. No File name Method Ident Vial Volume Dilution Amount Row number. Name of the chromatogram file (read-only). Name of the method file *.mtw used for recording the chromatogram (read-only). User defined identifier for chromatogram.
10 Batch reprocessing Sample Info 1 Sample Info 2 10.3.2 First sample description. Will be placed into appropriate passport field. 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.
11.1 Software license 11 Appendix 11.1 Software license As the purchaser of the «IC Net 2.0» PC software you also receive the license to use this software on your PC. The PC software has been validated by Metrohm in accordance with the requirements of the ISO 9001 quality system concerning its functioning, analytical performance and accuracy of results. The software functions are documented in the Software Manual provided. Please send us your 8.110.
11 Appendix 11.3 Index % %B .................................................................... 71,72 %C .................................................................... 71,72 %D .................................................................... 71,73 1 1st component....................................................... 110 1st peak ................................................................ 110 7 709 IC Pump advanced......................................................... 69 features....
11.3 Index ADC response ........................................................149 Add level ...............................................................126 ............................................................105 .........................................................52 ......................................36,37,45,46,61,63,73, ...........................................76,79,82,91,93,94,95 Adjusted volume ....................................................
11 Appendix Calibration graph size ............................................ 157 Chromatogram directory ........................................ 108 Calibration level .......................... 23,100,125,126,128, Chromatogram plot................................................ 133 ........................................... 159,164,167,172,175 Calibration method ................................................ 128 Calibration results .................................................
11.3 Index Control lines ............................................................89 Copy concentrations from level ...............................126 Copy to clipboard ...................................................130 Corr. .....................................................................127 Corrected retention time .........................................120 Correction factor ......................................................69 Correlation coefficient ....................................
11 Appendix Eluent B ................................................................ 103 Eluent C ................................................................ 103 Eluent report ....................................................... 132 Enable baseline penetration .................................... 119 Enable detection .................................................... 115 Enable negative peaks............................................ 115 Enable peak reject .....................................
11.3 Index I IC Applications Collection (8.732.2013)..................2 IC pump ..................................................................43 Icons 709 IC Pump ....................................................67 732 IC Detector................................................57 733 IC Separation Center ................................64 750 Autosampler..............................................83 752 Pump Unit .................................................74 753 suppressor Module............
11 Appendix M Main window elements ............................................................ 8 icons .................................................................. 9 Make report ............................................. 108,131,173 Manual ........................................... 75,78,81,84,88,90 Manual injection ...................................................... 86 Mark ....................................................................... 62 Master .....................................
11.3 Index P Packing material ....................................................102 ...........................................................157 Page margins.........................................................157 Paper size............................................................158 Parameter ..........................................91,93,94,95,109 Parity .................................................................33,39 Particle size ......................................................
11 Appendix R Rack definitions ....................................................... 92 Rack type ................................................................ 93 Range .......................................... 32,39,59,60,62,136 raw concentration .................................................. 142 Raw data ............................................................. 149 Raw data compression ........................................... 160 Raw data points .........................................
11.3 Index Save chromatogram after the run .............................108 Start delay ............................................................. 106 .....................................................153 Start determination .................................................. 22 Scaling chromatogram axes ...............................150 Scaling of X axis ..................................................154 Scaling of Y axis ..................................................
11 Appendix program ........................................................... 98 Valve position for rinse ............................................ 84 ValveA .................................................................... 62 ValveB .................................................................... 62 Verify sample .......................................................... 22 T Tab size ................................................................ 140 Tabulated calibration .................
