Page 1 Agilent 1100 Series Handheld Control Module User’s Guide...
Page 2 142 Reproduction, adaption, change without notice. or translation without Warning Symbols Used prior written permission Agilent Technologies In This Book is prohibited, except as makes no warranty of allowed under the any kind with regard to copyright laws.
Page 3 Agilent 1100 Series Handheld Control Module User’s Guide...
Page 4 HPLC using the control module, shown opposite. The control module provides complete local control and monitoring of a single module or an entire Agilent 1100 Series system. There is no data evaluation in the control module. The control module allows you to do a variety of HPLC tasks including automated sample preparation and injection, isocratic, gradient and multiple method analyses.
Page 5 In This Book Solvent cabinet Vacuum degasser Pump Control module Autosampler Column compartment Detector...
Page 6 In This Book...
Page 7 Part 1 “Using the Agilent 1100 Series Control Module” describes the control module, its features and its functionality. Part 2 “Using the Agilent 1100 Series Modules” describes how to use the individual HPLC modules to run isocratic, gradient and multiple-vial analyses using a single method or more than one method.
Page 8 In This Book...
Page 9: Table Of Contents
Control Module Keys 20 Control Module Software 24 Control Module Versions 31 2 Working with the Control Module How to use the Agilent 1100 Series control module 33 Installing the Control Module 34 General Functions 35 Troubleshooting 36 Inserting and Removing PC cards 37...
Page 10 Contents Part 2 Using the Agilent 1100 Series Modules 3 Using the Pump Operational details for the Agilent 1100 Series pumping systems 63 Turning the Pump On and Off 64 Entering Settings 64 Purging the Pump 64 Purging Procedure 65...
Page 11 Tracking Autosampler History / EMF limits 79 Resetting the Autosampler 80 Troubleshooting the Autosampler 80 6 Using the Manual Injection Valve Operational details for the Agilent 1100 Series manual injection valve 81 About the Injection Valve 82 Making An Injection 82...
Page 12 Tracking Column Compartment History 99 Tracking Column ID History 99 Resetting the Column Compartment 100 Part 3 Using the Agilent 1100 Series LC System With Control Module 9 Running an Isocratic Analysis How to analyze the Agilent Technologies isocratic standard sample us-...
Page 13 Saving Settings in a Method 106 Observing the Chromatogram 107 Starting the Analysis 108 10 Running a Gradient Analysis How to analyze the Agilent Technologies isocratic standard sample us- ing a gradient analysis 109 What You Will Need 110 Preparing the LC System 111...
Page 14 Contents 12 Running an Injector Program How to create an injector program 129 Creating an Injector Program 130 Entering Injector Program Settings 130 Saving the Method 131 Safety Information 142 Radio Interference 144 Agilent Technologies on Internet 145...
Page 15 Part 1 1 The Agilent 1100 Series Control Module 2 Working with the Control Module Part 1 Using the Agilent 1100 Series Control Module...
Page 16 Using the Agilent 1100 Series Control Module...
Page 17: The Agilent 1100 Series Control Module
The Agilent 1100 Series Control Module...
Page 18: Overview Over The Agilent 1100 Series Control Module
The Agilent 1100 Series Control Module Overview over the Agilent 1100 Series control module...
Page 19: Control Module Features
Control Module Features The control module provides complete local control and monitoring of a single module or an entire Agilent 1100 Series system. You have easy access on every supported function, you can easily control all parameters and settings and you can configure various communication channels with other devices, in order to comfortably analyze the generated data.
Page 20: Control Module Keys
The Agilent 1100 Series Control Module Control Module Keys Control Module Keys Figure 1 The Agilent 1100 Series Control Module Action keys execute specific operations and access Plot screen m (menu) key Navigation keys provides access different navigational software areas...
Page 21 The Agilent 1100 Series Control Module Control Module Keys The display will show you a variety of menu buttons [F1-F5] (in the lower section) or function buttons [F6-F8] (in the right hand section) that can be accessed with the corresponding Navigation (for menus) and Action (for functions) keys.
Page 22 The Agilent 1100 Series Control Module Control Module Keys • To move back to the previous information screen select the Previous button [F6]. The m (menu) key You can use the m (menu) key on the control module keyboard to access selected functionality quickly wherever you are in the software.
Page 23 The Agilent 1100 Series Control Module Control Module Keys Navigation keys These 5 keys [F1 - F5] allow you to switch between the menus. Within these menus the relevant parameters can be set and certain functions can be accessed. The Navigation keys always correspond to a button displayed above them on the screen.
Page 24: Control Module Software
The Agilent 1100 Series Control Module Control Module Software Figure 4 Keypad of the Control Module , ; : Control Module Software The Control Module User Interface In a basic configuration of modules there are at least three main screens, the Analysis, Status and System screens.
Page 25 The Agilent 1100 Series Control Module Control Module Software distinguish between the different modules in your system, or in the case of the Views button [F5], between screens. Analysis Screen The Analysis screen provides access to all LC analytical settings. The most commonly used settings are displayed with their corresponding set and actual values.
Page 26 The Agilent 1100 Series Control Module Control Module Software The screen provides access to: • Settings — all LC analytical system and module settings, • Timetable — time programmable settings, • Method — method management functions (load, save, delete), • Sequence — multiple method analyses, and •...
Page 27 The Agilent 1100 Series Control Module Control Module Software Figure 7 Where to go from the Analysis Screen - Menu Structure Analysis Start Plot Settings Timetable Method Sequence Views LC System Analysis Pump (Samples) Autosampler Setup Detectors System Col. Compartment...
Page 28 The Agilent 1100 Series Control Module Control Module Software System Screen The System screen provides access to non-routine settings and provides error checking, control, testing and tracking usage for LC system and modules. This screen displays the logbook together with the LC system and module status.
Page 29 The Agilent 1100 Series Control Module Control Module Software Figure 9 Where to go from the System Screen - Menu Structure System Start Plot Control Configure Tests Records Views LC System Analysis Pump (Samples) Autosampler Setup Detectors System Col. Comp.
Page 30 The Agilent 1100 Series Control Module Control Module Software Figure 10 Status Screen Samples Screen Operating from this screen you have easy access on the sample tray. Using the Vial Range function you can specify the vials you want to analyze and the desired method.
Page 31: Control Module Versions
The Agilent 1100 Series Control Module Control Module Versions Using the Direction and Selection keys of the control module you can change the scale of the plot window. With the Rescale button [F7] you can optimize the screen according to the selected signal and parameter ranges.
Page 32 The Agilent 1100 Series Control Module Control Module Versions...
Page 33: Working With The Control Module
Working with the Control Module How to use the Agilent 1100 Series control module...
Page 34: Installing The Control Module
LAN card. Connect the CAN (controller area network) connector of the control module cable to one of the two CAN connectors on one of the Agilent 1100 Series modules. Figure 13 Connecting the CAN Connector to Rear Panel...
Page 35: General Functions
Working with the Control Module General Functions General Functions Turning On/Off LC System and Modules Use the On/Off button [F7] in the Analysis screen to turn on or off either the complete system or each module individually. Setting Date and Time You can set the date and time using the context menu (m key) while the System screen is active.
Page 36: Troubleshooting
Troubleshooting the Control Module If your control module does not work correctly, disconnect the module CAN connector from the rear of the Agilent 1100 Series module it is attached to and reconnect it. If the problem still remains, then •...
Page 37: Inserting And Removing Pc Cards
3 To remove the PC card, press the card eject button on the left hand side of the module. NOT E Use only Agilent Technologies or SunDisk Corporation ATA Flashdisks, like the Agilent Technologies F1215C, F1013C or F1014C. Figure 14...
Page 38: Working With Methods
Working with the Control Module Working with Methods Working with Methods A method contains a complete set of injection, separation and detection parameters, including the timetable and injector program. Vial range information is not part of the method. There are two types of methods: •...
Page 39 Working with the Control Module Working with Methods when a module was added to or removed from the system. A partial method can not be loaded as the current method. Modifying a Method A method can be modified by changing the settings in the Analysis or Settings screens.
Page 40 Working with the Control Module Working with Methods NOT E The left arrow key can be used as backspace, the right arrow key is used to move to the next character position. Protecting a Method To protect the current method. 1 Select the Method button [F3] in the Analysis screen.
Page 41 Working with the Control Module Working with Methods To save the current method: 1 Select the Method button [F3] in the Analysis screen. 2 Select Save As using the Action keys. 3 Enter a name as described in “Specifying a Method Name” on page 39, or simply continue with the next step if you want to keep the current method name.
Page 42 Working with the Control Module Working with Methods 1 Insert the PC card into the control module as described in “Inserting and Removing PC cards” on page 37. NOT E Methods from a freshly installed PC card are not available. Restart the control module using the Restart function via the m (menu) key from the main screens.
Page 43: Time Programming
Working with the Control Module Time Programming 4 Restart the control module using the Restart function via the m (menu) key (available from the main screens). 5 Load the method from the PC card. See section “Exchanging Methods With the PC Card”...
Page 44: Automating Analyses
Working with the Control Module Automating Analyses You can edit an existing timetable line by pressing the Enter key. Use the Delete button [F6] and make a choice from the pop-up menu to delete either the selected line or the whole timetable. You can copy and paste timetable lines by selecting the respective choices available from the context menu (m key).
Page 45 Working with the Control Module Automating Analyses • Line Number Starting with 1 the sequence lines are automatically counted up. • Vial Range Information Just like in the Analysis screen you can specify a range of vials together with the number of injections per vial.
Page 46: Displaying Data Graphically
Working with the Control Module Displaying Data Graphically Displaying Data Graphically Using the Plot screen you have many opportunities to display a wide variety of signals on a graphic display while the analysis is performed. Selecting Signals Among all the signals available up to 3 can be chosen for graphical display. 1 From the Plot screen press the Select button [F6] to show the Plot selection menu.
Page 47 Working with the Control Module Displaying Data Graphically Y (signal unit) axis To rescale the Y (signal unit) axis there are several possibilities: • From the Plot Selection windows (available from the Plot screen via the Select button [F6]) choose a signal from either list box and press the Setup button [F7]. You can specify a Y range separately for each signal.
Page 48: Logbooks
Working with the Control Module Logbooks Logbooks The control module keeps track of all kinds of system parameter changes, error messages and maintenance data. You can access the logbooks by pressing the Records button [F4] in the System screen. Information on this screen includes the module product and serial number, firmware version number and the operation time from power-on until now.
Page 49: Printing Screens
NOT E A converter from a serial (RS-232) to a parallel (Centronics) connection is available from Agilent Technologies, part number 5181-1529. You can configure the printer by pressing the Configure button [F2] in the System screen and then selecting LC System. In the following Config screen press the Printer button [F1] to open the respective dialog.
Page 50 Working with the Control Module Printing Screens Print Plot In the Plot screen you can create a screen hard copy using the m (menu) key and selecting Print Plot from the context menu. The printout will also include a legend and the date and time.
Page 51: Connecting External Devices
Working with the Control Module Connecting External Devices Connecting External Devices There are several kinds of interfaces that enable the Agilent 1100 Series modules to communicate with a range of other output devices. For some of them extra hardware needs to be installed.
Page 52 Working with the Control Module Connecting External Devices Ready When all Agilent 1100 Series modules are ready for the next analysis, this signal is on. Other modules or external devices now can react (e.g. by issuing a start request). Prepare This causes the modules to get ready for the next analysis (e.g.
Page 53: Firmware
Working with the Control Module Firmware If the appropriate extension board is part of your system, you can use this output to inform external devices about the vial number currently processed. External Contacts With an optional external contacts board you can use various opportunities to synchronize LC activities with external devices.
Page 54: Updating Firmware In The Lc Modules
Working with the Control Module Updating Firmware in the LC Modules 4 Switch on the component where the control module is plugged in. 5 In the System screen press Records. 6 Choose Controller from the list. If the version number on the display is lower than the current number start the update by pressing FW Update.
Page 55 The LC modules can also be updated via the firmware upgrade utility delivered with Agilent ChemStation. Update Functions for Agilent 1100 Series modules Select File Allows to select the file on the PC card for the module that is updated with new firmware.
Page 56 Working with the Control Module Updating Firmware in the LC Modules Preparing Firmware Update 1 Isolate the module you want to update with new firmware by switching off all other modules or by disconnecting all other CAN cables. Remove the GPIB cable from the rear of the module.
Page 57 Working with the Control Module Updating Firmware in the LC Modules 4 Select the file for the update (RESXXX.DLB), press the Execute button [F8] and confirm with Yes. In the screen you can monitor the status of the update procedure. 5 When the status bar has reached 100% press the Esc key.
Page 58: Coexecution With Agilent Chemstation
Features • Both user interfaces, the control module and the Agilent ChemStation, can be connected to a Agilent 1100 Series system at the same time. • Parameter entry is possible from both user interfaces. Parameters will be updated on the other user interface within a few moments.
Page 59 Working with the Control Module Coexecution with Agilent ChemStation this specific entry field is disabled on the control module. • If an analysis is running with the control module, the Agilent ChemStation should not be turned on or rebooted. • If the Agilent ChemStation starts an analysis, the control module is the slave/ monitor system.
Page 60 Working with the Control Module Coexecution with Agilent ChemStation...
Page 61 Part 2 3 Using the Pump 4 Using the Degasser 5 Using the Autosampler 6 Using the Manual Injection Valve 6 Using the Manual Injection Valve 7 Using the Detectors 8 Using the Column Compartment Part 2 Using the Agilent 1100 Series Modules...
Page 62 Using the Agilent 1100 Series Modules...
Page 63: Using The Pump
Using the Pump Operational details for the Agilent 1100 Series pumping systems...
Page 64: Turning The Pump On And Off
Using the Pump Turning the Pump On and Off Turning the Pump On and Off To turn the pump on or off you can use the On/Off button [F7] in the Analysis or System screen: 1 Enter the Analysis or System screen. 2 Select the On/Off button [F7].
Page 65: Purging Procedure
Using the Pump Purging Procedure Purging Procedure 1 Ensure that an outlet tube is connected from the purge valve to a waste solvent bottle. 2 Open the purge valve. 3 Enter the Analysis screen. 4 Set the purge flow rate in the regular flow rate section of the Analysis screen, for example, to 5 ml/min.
Page 66: Adjusting Compressibility
Using the Pump Adjusting Compressibility Adjusting Compressibility Liquid chromatographic solvents are compressible under pressure. This solvent compressibility produces a change in flow rate as the pressure changes. To compensate for this effect, you can use the pump compressibility setting to maintain a uniform and accurate flow regardless of the system pressure.
Page 67: Adjusting Stroke Volume
Using the Pump Adjusting Stroke Volume When the compressibility setting is set to Off, the pump makes no compensation for the compressibility of the mobile phase. For each particular compressibility value, the piston stroke (distance piston moves) and the speed at which the piston moves are adjusted accordingly, compensating for the solvent compressibility.
Page 68: Troubleshooting The Pump
2 Select Pump from the menu. You can now select various tests to check the pump. For further information about these tests see the Reference Manual for the Agilent 1100 Series pump. Tracking Pump History / Pump EMF Limits 1 Select the Records button [F4] in the System screen.
Page 69: Resetting The Pump
Using the Pump Resetting the Pump Resetting the Pump 1 Select the Control button [F1] in the System screen. 2 Select Pump from the menu. 3 Press the Enter key. 4 Select the Reset button [F7] to stop the pump operation and perform a hardware initialization.
Page 70 Using the Pump Resetting the Pump Settings...
Page 71: Using The Degasser
Using the Degasser Operational details for the Agilent 1100 Series vacuum degasser...
Page 72: Starting The Degasser
Using the Degasser Starting the Degasser Starting the Degasser 1 Press the line-power switch on the front panel. 2 Turn on your pump by selecting the On/Off button [F8] in the Analysis screen. 3 Observe the degasser status lamp on the front panel. The status lamp is off when there is sufficient vacuum in the degasser.
Page 73: Changing Solvents
Using the Degasser Changing Solvents Changing Solvents If you are changing to a solvent that is immiscible with the solvent currently in the tubing: 1 Replace the current solvent: with iso-propanol, if current solvent is organic, or with water, if current solvent is an organic buffer or salt. 2 Flush the online degasser and all tubing thoroughly.
Page 74 Using the Degasser Changing Solvents...
Page 75: Using The Autosampler
Using the Autosampler Operational details for the Agilent 1100 Series autosampler...
Page 76: Configuring The Autosampler
Using the Autosampler Configuring the Autosampler Configuring the Autosampler 1 Select the Configure button [F2] in the System screen. 2 Select Autosampler from the menu. 3 Press the Enter key. You can configure the syringe volume, seat capillary volume, action on missing vial, trays, interfaces etc.
Page 77 Using the Autosampler Entering Settings More specific settings (draw speed, eject speed, draw position offset) can be entered using the More... button [F1] and choosing the Settings option. Setting the Injection Mode There are two modes which can be set: •...
Page 78 Using the Autosampler Entering Settings runtime. The injection cycle will not be started. This procedure reduces the total injection time without interfering with the current run. By choosing the Overlap Injection Cycle option the next vial will be placed in the injection port after the selected elapsed runtime.
Page 79: Aligning Transport Arm/Gripper
Using the Autosampler Aligning Transport Arm/Gripper Aligning Transport Arm/Gripper 1 Press the Tests button [F3] in the System screen. 2 Choose Autosampler from the list. 3 Press the Align button [F1]. 4 Choose Transport. 5 Enter the desired values in the corresponding fields. The field X Correction sets the default value for the axis parallel to the front panel (left-right motion).
Page 80: Resetting The Autosampler
The injector step functions can be used in troubleshooting to check the single steps of the injection cycle. For a complete description of each step, see the Reference Manual for the Agilent 1100 Series autosampler. If you have a thermostatted autosampler, you can also test the auxiliary signals by pressing the Signal button in the Test screen.
Page 81: Using The Manual Injection Valve
Using the Manual Injection Valve Operational details for the Agilent 1100 Series manual injection valve...
Page 82: About The Injection Valve
Using the Manual Injection Valve About the Injection Valve About the Injection Valve The injection valve has six ports and can be moved manually between two positions. In the LOAD position, the mobile phase is led from the pump directly to the column, allowing you to inject your sample into the sample loop.
Page 83: Completely Filling The Sample Loop
Using the Manual Injection Valve Completely Filling the Sample Loop Completely Filling the Sample Loop This is the conventional method in which an excess of sample is used to fill the sample loop completely. The volume of the loop determines the injection volume. 1 Fill syringe with sample.
Page 84: How Much Sample Is Actually Injected
Using the Manual Injection Valve How Much Sample Is Actually Injected? 5 Slowly inject sample. 6 Leave syringe in position and move valve to INJECT position. 7 Remove syringe. How Much Sample Is Actually Injected? When the sample loop is completely filled, the amount of sample injected is equal to the volume of the sample loop plus the volume of the valve passages (1 in rotor and 2 in stator).
Page 85: An Alternative Way To Fill The Loop
Using the Manual Injection Valve An Alternative Way to Fill The Loop An Alternative Way to Fill The Loop When the sample loop is completely filled you can either inject the sample into the loop or use the syringe to draw the sample through the loop. 1 Move valve to LOAD position.
Page 86 Using the Manual Injection Valve An Alternative Way to Fill The Loop...
Page 87: Using The Detectors
Using the Detectors Operational details for the Agilent 1100 Series variable wavelength, multiple wavelength, refractive index, fluorescence light, and diode array detectors...
Page 88: Turning The Lamp On And Off
Using the Detectors Turning the Lamp On and Off Turning the Lamp On and Off To turn the lamp on and off use the On/Off button [F7] in the Analysis screen: 1 Enter the Analysis screen. 2 Select the On/Off button [F7]. 3 Select the Lamp button [F6].
Page 89 Using the Detectors Entering Settings settings and the margin for negative absorbance. The option Spectrum allows you to enter a wavelength range for a sample spectrum. Fluorescence Light Detector For the fluorescence light detector the following settings can be entered: Excitation wavelength, emission wavelength and Multi wavelength settings can be set in the regular Settings screen.
Page 90: Resetting The Baseline
Using the Detectors Resetting the Baseline Resetting the Baseline You can reset the baseline using the Balance button [F1] (Zero button [F1] when using the Refractive Index Detector) in the Detector Control screen. Please note that this procedure is not available for the Fluorescence Light Detector: 1 Select the Control button [F1] in the System screen.
Page 91: Troubleshooting The Detector
Using the Detectors Troubleshooting the Detector Troubleshooting the Detector 1 Select the Tests button [F3] in the System screen. 2 Select the Detector from the menu. 3 Press the Enter key. 4 Select the test you require. The selection of tests depends on the. For information about each test, see the Reference Manual for the Agilent 1100 detectors.
Page 92: Resetting The Detector
Using the Detectors Resetting the Detector Resetting the Detector 1 Select the Settings button [F1] in the Analysis screen. 2 Select the Detector from the menu. 3 Press the Enter key. 4 Select the Default button [F7] to reset the detector settings to their default values. Lamp Ignition Routine (VWD only) When the lamp is turned on, the following routine is implemented: •...
Page 93 Using the Detectors Configuring the Analog Channel Output Wavelength Detector and Refractive Index Detector have one) at the back side of the module. To configure the analog outputs: 1 Press the Settings button [F1] in the Analysis screen. 2 Choose the detector and press enter. 3 Press the Analog button [F3].
Page 94 Using the Detectors Configuring the Analog Channel Output...
Page 95: Using The Column Compartment
Using the Column Compartment Operational details for the Agilent 1100 Series thermostatted column compartment...
Page 96: Turning The Column Compartment On And Off
Using the Column Compartment Turning the Column Compartment On and Off Turning the Column Compartment On and Off You can turn the column compartment on and off by using the On/Off button [F7] in the Analysis screen: 1 Enter the Analysis screen. 2 Select the On/Off button [F7].
Page 97: Configuring The Column Compartment
Using the Column Compartment Configuring the Column Compartment Configuring the Column Compartment 1 Select the Configure button [F2] in the System screen. 2 Select Column Comp from the list. 3 Press the Enter key. You can now configure the leak-detection mode, temperature-on at power-on, the interfaces and the column identification module.
Page 98: Selecting Separated Or Combined Mode
Using the Column Compartment Selecting Separated or Combined Mode Selecting Separated or Combined Mode This mode allows the temperature setting of both heaters independent from each other. If not enabled both heaters are kept on the same temperature. 1 Select the Settings button [F1] in the Analysis screen. 2 Select Column Comp from the menu.
Page 99: Troubleshooting The Column Compartment
You can select the Calibrate test to check the operation of the Column Compartment. For information about the test, see the Reference Manual for the Agilent 1100 Series column compartment. Tracking Column Compartment History 1 Select the Records button [F2] in the System screen.
Page 100: Resetting The Column Compartment
Using the Column Compartment Resetting the Column Compartment By selecting the More ... button [F1] you can enter values and check a variety of features for the installed column. For example, the maximum pressure allowed and the maximum recommended temperature. You can check the number of injections that have been made on the column.
Page 101: Part 3 Using The Agilent 1100 Series Lc System With Control Module
Part 3 9 Running an Isocratic Analysis 10 Running a Gradient Analysis 11 Running Multiple-Vial Analyses 12 Running an Injector Program Part 3 Using the Agilent 1100 Series LC System With Control Module...
Page 102 Using the Agilent 1100 Series LC System With Control Module...
Page 103: Running An Isocratic Analysis
Running an Isocratic Analysis How to analyze the Agilent Technologies isocratic standard sample using a single injection analysis...
Page 104: What You Will Need
5 Allow the detector at least 15 minutes to provide a stable baseline. 6 Fill the contents of a Agilent Technologies isocratic standard sample ampoule into a vial and seal the vial with a cap. Place the vial in position 1 of the autosampler tray.
Page 105: Entering Settings
Running an Isocratic Analysis Entering Settings Entering Settings To set up the isocratic analysis you will set the LC system settings to default and then modify selected settings, the other settings will remain with their default values. You will then save these settings to a method called ISO. 1 Enter the Analysis screen.
Page 106: Saving Settings In A Method
Running an Isocratic Analysis Saving Settings in a Method Table 2 Values in Analysis Screen Setting Value Detection wavelength 254 nm Injection volume 1 µl Stoptime 6 min Saving Settings in a Method 1 Select the Method button [F3] in the Analysis screen. 2 Select the Save As button [F8].
Page 107: Observing The Chromatogram
Running an Isocratic Analysis Observing the Chromatogram Observing the Chromatogram 1 Select the Plot button [F6] in the Analysis screen. 2 Press the Select button [F6]. 3 Choose a Signal from the Available Signals list box. 4 Press the Enter key NOT E You can choose several signals at a time.
Page 108: Starting The Analysis
Running an Isocratic Analysis Starting the Analysis Figure 16 Figure 16 Analysis of Isocratic Standard Sample Analysis of Isocratic Standard Sample Starting the Analysis NOT E The analysis can be started from various other screens, e.g. System, Status, Sampels or Sequence screen. 1 Enter the Analysis screen.
Page 109: Running A Gradient Analysis
Running a Gradient Analysis How to analyze the Agilent Technologies isocratic standard sample using a gradient analysis...
Page 110: What You Will Need
Running a Gradient Analysis What You Will Need What You Will Need Instruments Agilent 1100 Series binary or quaternary pump, autosampler, UV-detector and degasser. Column A 125 mm × 4.0 mm Hypersil ODS, 5 µm (Agilent Technologies part number 7982618-564).
Page 111: Preparing The Lc System
5 Allow the detector at least 15 minutes to provide a stable baseline. 6 Fill the contents of a Agilent Technologies isocratic standard sample ampoule into a vial and seal the vial with a cap. Place the vial in position 1 of the autosampler tray.
Page 112 Running a Gradient Analysis Entering Settings 1 Enter the Analysis screen. 2 Set the Vial Range as 1 to 1. 3 Set the Number of Injections to 1. 4 Skip the method name field 5 Select the Settings button [F1]. 6 Select LC System from the menu.
Page 113 Running a Gradient Analysis Entering Settings 13 Select the Pressure button. 14 Set the upper pressure limit to 400 bar. 15 Select the Done button. 16 Select the Timetable button. 17 Select the Insert button. 18 Enter a value of 2 minutes and select Composition as the setting. If you have a quaternary pump, set the %B composition to 65, %C and %D to 0.00.
Page 114: Saving Settings In A Method
Running a Gradient Analysis Saving Settings in a Method Saving Settings in a Method 1 Select the Method button [F3] in the Analysis screen. 2 Select the Save As button [F8]. 3 Enter the method name as GRAD using the selection keys (also see “Specifying a Method Name”...
Page 115 Running a Gradient Analysis Observing the Chromatogram A typical gradient chromatogram for this analysis is shown in Figure 17. Figure 17 Gradient Analysis of Isocratic Standard The exact profile of the chromatogram will depend on the column you have used. Differences in retention times and areas of the peaks in your chromatogram and the one shown in Figure 17 might be a result of variations in the concentration of the sample from batch to batch, the quality of the solvents used and the column...
Page 116: Starting The Analysis
Running a Gradient Analysis Starting the Analysis Starting the Analysis NOT E The analysis can be started by pressing the Start button [F8] from the Samples screen, the System screen, or the Status screen. 1 Enter the Analysis screen. 2 Select the Start button [F8]. 3 Select OK to confirm the vial range and injection number and press the Enter key to start the analysis.
Page 117: Running Multiple-Vial Analyses
Running Multiple-Vial Analyses How to setup multiple vial analyses using the same method and different methods...
Page 118: Analyzing Multiple Vials Using The Same Method
Running Multiple-Vial Analyses Analyzing Multiple Vials Using the Same Method Analyzing Multiple Vials Using the Same Method This section describes how to set up a 25-vial analysis with one injection from each vial. You will use a previously created method. The samples are located in positions 1 to 25 of the autosampler tray.
Page 119 Running Multiple-Vial Analyses Analyzing Multiple Vials Using Different Methods The example assumes that the sequence table is empty. If the sequence table is not empty, use the All Lines item, accessed by pressing the Delete button [F6]. 1 Select the Sequence [F4] in the Analysis screen. 2 For sequence line 1, select the Insert button [F7] and enter: Vial Range 1 to 20...
Page 120: Single-Level Calibration Sequences
Running Multiple-Vial Analyses Single-Level Calibration Sequences 7 Select the Done button [F6] to enter sequence line 3 settings and complete the sequence. 8 Select the Start button [F8] in the Sequence screen. 9 Select the OK button to start the sequence. Single-Level Calibration Sequences The following procedure describes how to set up a calibration sequence for an analysis which uses single-level calibration.
Page 121: Multiple-Level Calibration Sequences
Running Multiple-Vial Analyses Multiple-Level Calibration Sequences 3 Select the Calibration button [F1] to display the Calibration Settings screen for sequence line 1 and choose Edit. 4 Enter the following information: Calibration vial range 90 to 90 Number of injections Calibration method METH1 Recalibrate every 2 vials multi...
Page 122 Running Multiple-Vial Analyses Recalibrating With the Same Group of Standards • each sample is analyzed once, • the calibration standards are analyzed twice before the samples and re-analyzed twice after every 5 samples, C1 C2 C3 S10-S14 C1 C2 C3 S15-S19 C1 C2 C3 S20-S24 C1 C2 C3 •...
Page 123: Recalibrating With Multiple Groups Of Standards
Running Multiple-Vial Analyses Recalibrating With Multiple Groups of Standards • the three calibration standards in duplicate, • sample vials 10 through 14, • the three calibration standards in duplicate, • sample vials 15 through 19, • the three calibration standards in duplicate, •...
Page 124 Running Multiple-Vial Analyses Recalibrating With Multiple Groups of Standards C1 C2 C3 S13-S15 C1 C2 C3 S16-S18 C1 C2 C3 S19-S21 C1 C2 C3 • the calibration standards of type B are in positions 4, 5 and 6 of the autosampler tray and the 9 sample vials are in positions 13 to 21, and •...
Page 125 Running Multiple-Vial Analyses Recalibrating With Multiple Groups of Standards Inj. Volume Default Method METH2 8 Select the Calibration button [F1] to display the Calibration Settings screen for sequence line 2 and choose Edit. 9 Enter the following information: Calibr. vial range 4 to 6 #Inj Inj.
Page 126: Synchronizing Analyses With External Devices
Running Multiple-Vial Analyses Synchronizing Analyses with External Devices • three type B calibration standards in duplicate. Synchronizing Analyses with External Devices With an APG remote connector the system can be connected to external devices in order to synchronize the analyses. This is necessary when an external device needs some time in order to get ready for a new analysis and when transmitting of a start request is required (see “Connecting External Devices”...
Page 127 Running Multiple-Vial Analyses Synchronizing Analyses with External Devices Figure 18 Send single external start request In this mode the control module will simply track the progress of the vial range or sequence. It will indicate the proper sample, change sequence lines, load methods or other sequence related actions for each run.
Page 128 Running Multiple-Vial Analyses Synchronizing Analyses with External Devices Figure 20 Wait for single external start request Wait for Repeated Start Request After pressing the Start button [F8] the autosampler will wait for external start requests before each vial in the range or sequence. They have to be generated by the external device.
Page 129: Running An Injector Program
Running an Injector Program How to create an injector program...
Page 130: Creating An Injector Program
Running an Injector Program Creating an Injector Program Creating an Injector Program The injector program is part of the method. The injector program screen can be accessed using the Inj. Program button [F3] in the Autosampler Settings screen. This section describes an injector program to do sample preparation involving a precolumn derivatization reaction.
Page 131: Saving The Method
Running an Injector Program Saving the Method 6 Select the Settings button [F1]. 7 Select Autosampler from the menu. 8 Select the Inj.Program button [F3] to display the Program screen. 9 For program line 1, select the Insert button [F7]. 10 Select the DRAW function and enter the draw settings as described in Table 4.
Page 132 Running an Injector Program Saving the Method Table 4 Injector Program Lines Line Function Parameters Comment DRAW 2 µl (AMOUNT) from Draw 2 µl from air into the needle Air (SOURCE) capillary, to separate the mobile phase sitting in the capillary from the sample.
Page 133 Index draw speed, 77 calibration, 44 action key, 23 eject speed, 77 column ID, 97 active signal, 47 entering settings, 76 column switch, 98 add button, 35, 48 external contacts, 76 configure, 36 adjusting view, 35 injection modes, 77 copy >>, 42 Agilent ChemStation, 51 injection volume, 76 cursor, 47...
Page 134 Index temp, 96 Agilent ChemStation, 58 peakwidth, 88 tests, 68, 79, 80, 91, 99 available modules, 35 resetting, 92 timetable, 26, 43 coexecution, 58 resetting the baseline, 90 transfer, 55 contrast, 35 settings, 88 views, 24, 25, 26 display, 35 slit width, 88 write, 97 displayed modules, 35...
Page 135 Index operation firmware, 57 ID tag, 97 variable wavelength detector, 88 preparing, 56 identify button, 48 LC system resident, operation, 54 identify modules, 48 configuring, 36 select file, 55 initialize, 42 firmware update, 54 switching modes, 56 injection mode, 77 general functions, 36 transfer, 55 injection valve...
Page 136 Index user ID, 41 page layout, 49 on/off, 64 working with, 38 paper size, 49 piston, 67 method button, 38 parameter changes, 48 purging, 64 MIO interface, 51 partial method, 38 resetting, 69 missing vial, 76 PC card resetting settings, 69 modifying a method, 39 initialize, 42 settings, 64...
Page 137 Index RS232 interface, 51 refractive index detector, 89 time and date, 35 running an analysis, 103 settings button, 25, 39 time axis, 46 running injector program, 129 setup button, 35, 46, 50 time programming, 43 setup logbooks, 48 timeout, 36 setup view, 35 timetable, 26, 43 sample...
Page 138 88 wavelength calibration, 92 version number, 56 checking, 56 views, 26 views button, 24, 25 warranty responsibility of Agilent Technologies, services, 141 statement, 139 wash mode, 77 wash vial, 77 washing the needle, 77 wavelength calibration, 92 wear count, 68...
Page 139 Warranty Statement All Chemical Analysis Products Agilent Technologies warrants its chemical analysis products against defects in materials and workmanship. For details of the warranty period in your country, call Agilent. During the warranty period, Agilent will, at its option, repair or replace products which prove to be defective.
Page 140 Warranty Statement product, 5 improper site preparation and maintenance, or 6 customer induced contamination or leaks. THE WARANTY SET FORTH IS EXCLUSIVE AND NO OTHER WARRANTY, WHETHER WRITTEN OR ORAL, IS EXPRESSED OR IMPLIED. AGILENT SPECIFICALLY DISCLAIMS THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE.
Page 141 Warranty Statement Responsibilities of Agilent Technologies Agilent Technologies will provide warranty services as described in Table 5. Table 5 Warranty Services Services During Warranty Warranty Period Type Agilent 1100 Series of Modules 1 Year Onsite GC, LC, UV-Visible, and LAS supplies...
Page 142: Safety Information
Safety Information Safety Information The following general safety precautions must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Agilent Technologies assumes no liability for the customer’s failure to comply with these requirements.
Page 143 Safety Information Do not operate the instrument in the presence of flammable gases or fumes. Operation of any electrical instrument in such an environment constitutes a definite safety hazard. Do not install substitute parts or make any unauthorized modification to the instrument.
Page 144: Radio Interference
Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations. Test and Measurement...
Page 145: Agilent Technologies On Internet
Agilent Technologies on Internet Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at: http://www.agilent.com Select “Products”- “Chemical Analysis”...
Page 146 Agilent Technologies on Internet...
Page 148 In This Book This book provides information about the control module and how to operate the Agilent 1100 Series modules and system for HPLC. • The Agilent 1100 Series Control Module • Working with the Control Module • Using the Pump •...

Agilent Technologies 1100 Series User Manual

1 The Agilent 1100 Series Control Module

2 Working with the Control Module

3 Using the Pump

4 Using the Degasser

5 Using the Autosampler

6 Using the Manual Injection Valve

7 Using the Detectors

8 Using the Column Compartment

Part 3 Using the Agilent 1100 Series LC System with Control Module

9 Running an Isocratic Analysis

10 Running a Gradient Analysis

11 Running Multiple-Vial Analyses

12 Running an Injector Program

Quick Links

Troubleshooting

Related Manuals for Agilent Technologies 1100 Series

Summary of Contents for Agilent Technologies 1100 Series

Table of Contents