1. Manuals
  2. Brands
  3. Gilson Manuals
  4. Security Sensors
  5. 155
  6. User manual

Gilson 155 User Manual

Uv/vis detectors
Hide thumbs
Table of Contents

Advertisement

Quick Links

Download this manual
sales@artisantg.com
artisantg.com
(217) 352-9330 |
|
Click HERE
Find the Gilson 100326 at our website:

Advertisement

Table of Contents
loading

Related Manuals for Gilson 155

Summary of Contents for Gilson 155

  • Page 1 (217) 352-9330 | Click HERE Find the Gilson 100326 at our website:...
  • Page 2 Gilson 155/156 UV/VIS Detectors User’s Guide LT1034/©2004 Gilson, Inc. All rights reserved March 2004 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 3 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 4: Table Of Contents

    Table of Contents Declaration of Conformity 1 Introduction Description ................1-1 Optics ................1-2 Display ................1-2 Features ................1-2 Unpacking ................1-3 Customer Service ..............1-4 Technical Specifications ............. 1-5 Modes and Their Parameters ..........1-9 Single Wavelength Mode ..........1-9 Dual Wavelength Mode ..........
  • Page 5 3 Operation Operation Flowchart ............3-2 Front Panel Diagram ............3-4 Software Structure .............. 3-6 Mode Selection ............... 3-6 Parameter List ..............3-6 Start Up ................. 3-12 Wake-Up Displays ............3-12 Selecting the Mode ............3-14 Error Messages ............... 3-15 Detector Setup Parameters ..........
  • Page 6 Peaks Too Broad ............5-7 Decreased Response to Known Sample ....5-7 Abnormally High System Pressure ......5-7 Diagnostics ................5-8 Numeric Analyses on the 155 Detector ....5-8 Repair and Return Policies ..........5-10 Telephone Numbers ............5-10 Before Calling Us ............5-10 Warranty Repair ............
  • Page 7 Appendix B Mode-Specific Functions Mode-Specific Output Channels ........B-1 Mode-Specific Remote Event and Autozero Functions ............. B-1 Appendix C Sensitivity Appendix D GSIOC Control GSIOC Commands .............. D-2 FIFO Commands ..............D-2 GSIOC Command List ............D-2 FIFO Command List ............D-11 Appendix E Replacement Parts Lamp Assemblies ..............

  • Page 8: Declaration Of Conformity

    EN61326, EN61000-3-3, EN61000-3-2, EN61010-1:2001 Manufacturer’s Name ........... Gilson, Inc. Manufacturer’s Address ........3000 W. Beltline Highway Middleton, WI 53562 EC Office Address ..........Gilson S.A.S. 19 Avenue des Entrepreneurs, B.P. 145 F-95400 Villiers-le-Bel, France Type of Equipment ..........Laboratory Equipment Model.
  • Page 9 EN61326, EN61000-3-3, EN61000-3-2, EN61010-1:2001 Manufacturer’s Name ........... Gilson, Inc. Manufacturer’s Address ........3000 W. Beltline Highway Middleton, WI 53562 EC Office Address ..........Gilson S.A.S. 19 Avenue des Entrepreneurs, B.P. 145 F-95400 Villiers-le-Bel, France Type of Equipment ..........Laboratory Equipment Model.

  • Page 10: Introduction

    Gilson modular HPLC system. And, the 155 Detector with its front panel control is also compatible with other commercially available HPLC systems. The 155 Detector can be controlled via its front panel or via external software, such as Gilson UniPoint™ System Software. The 156 Detector must be controlled via external software since it does not have an integral front panel display.

  • Page 11: Optics

    190 to 700 nm. The detector has a sensitivity range of 0.001 to 2.0 AUFS (Absorbance Units, Full Scale). Display Gilson designed the 155 Detector software to be completely self-guiding. All parameters, values and commands appear on the four-line display.

  • Page 12: Unpacking

    Introduction Unpacking Unpack the detector and its accessories carefully from the carton. Open the detector door and remove the foam insert from inside the detector. Cross-check the contents against the checklist below and against your packing slip, to verify that all parts are included and undamaged.

  • Page 13: Customer Service

    Introduction Customer Service Gilson, Inc., and its worldwide network of authorized representatives provide customers with these types of assistance: sales, technical, applications, and instrument repair. If you need assistance and are in the United States, contact your Gilson representative or call the Gilson Customer Service Department, toll-free at 800-445-7661 or call 608-836-1551.

  • Page 14: Technical Specifications

    Introduction Technical Specifications Warning: Changes or modifications to this device not expressly approved by Gilson could void the warranty. Note: This device has been tested and found to comply with the limits for a Class A digital device, pursuant to Part 15 of the FCC commercial environment.
  • Page 15 Introduction Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 16 Introduction Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 17 Introduction Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 18: Modes And Their Parameters

    Introduction Modes and Their Parameters The available modes and their parameters are described below. Single Wavelength Mode Wavelength, Sensitivity 1, Sensitivity 2, Peak width Dual Wavelength Mode Wavelength 1, Wavelength 2, Sensitivity 1, Sensitivity 2, Peak width, Ratio multiplier, Ratio Threshold Scan Wavelength Mode Wavelength (to monitor before and after the scan),...
  • Page 19 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 20: Installation

    Installation Operating Environment You can use the detector in normal laboratory and cold room environments. The factors described below will influence the performance of your detector. Temperature Changes in ambient temperature can produce noticeable output variations, especially at higher sensitivities. Avoid areas which are in direct sunlight for part of the day and those which are subject to draft;...

  • Page 21: Electrical Setup

    • turn on power You can also make these optional connections: • bidirectional communication with a Gilson system controller on the Gilson Serial Input/ Output Channel (GSIOC) • remote contact control functions The essential and optional setups are described in detail on the following pages.

  • Page 22: Rear Panel Diagram

    SW1 selector For reviewing and changing the unit ID. SW2 selector For reviewing and changing the baud rate. GSIOC Gilson Serial Input/Output Channel, a 2-way communications link to the computer. RS-232 Serial connector, a 2-way communications link to the computer.

  • Page 23: Essential Setup

    2-3. Output connections Note: If the detector is part of a Gilson HPLC system, you do not need to make output connections. Instead make the GSIOC connection between the detector and system controller as described in Optional Connections, page 2-6.
  • Page 24 • GSIOC connection • RS-232 connection • contact connections Note: You must connect the GSIOC cable if you use the detector as a data acquisition device in a Gilson HPLC system. If you won’t need the optional connections, proceed with Plumbing Setup page 2-12.

  • Page 25: Optional Connections

    Installation Optional Connections GSIOC connection If the detector is part of a Gilson HPLC system, the GSIOC port is used to transfer information between the detector and computer. The detector, and other Gilson GSIOC devices, can convert the RS-232 signal levels used by computers to the RS-422/485 signal levels required by the GSIOC and vice versa.
  • Page 26 Installation RS-232 connection If the detector is not part of an HPLC system controlled by Gilson software, the RS-232 port can be used to transfer information between the detector and a computer. Be sure your computer is turned off before making any connections.
  • Page 27 You can make contact connections from: • Microsoft Windows-based computer via Gilson 506 contact outputs • Gilson sampling injector, which acts as a controller of an isocratic auto-analytical system • Gilson fraction collector • Some Gilson pumps You can specify the timing of contact events from the Gilson control software.
  • Page 28 In single and dual wavelength modes: • a remote event contact causes a negative spike to appear in the analog output If the event is sent via the GSIOC to Gilson control software (using a Gilson 506C System Interface), a positive spike or event mark appears on the time line.

  • Page 29: Unit Id And Baud Rate Selection

    GSIOC commands to the detector via the GSIOC or RS-232 cable connection. At the factory, Gilson set the unit ID to 16. There is no need to change this number unless it is the same as that assigned to another Gilson instrument that is also connected along the GSIOC.

  • Page 30: Baud Rate

    As a default, the baud rate is set to “External,” indicating that the detector is a slave device in a Gilson system and the baud rate is being clocked outside of the detector. Other baud rate selections are available if the detector is being controlled by non-Gilson applications.

  • Page 31: Plumbing Setup

    Installation Plumbing Setup The detector arrives with the flow cell, the inlet and outlet tubing, and the end fittings already in place. You must make these two plumbing connections: Inlet tubing to your column outlet. See Inlet Tubing, below, for details. Outlet tubing to another detector or to a back pressure regulator if effluent is being directed to a fraction collector or to drain.

  • Page 32: Outlet Tubing

    Installation Capillary For the capillary flow cell the inlet and outlet capillaries are interchangeable. Designate one of the capillaries as the inlet and connect it to the column outlet using the fitting from the accessory package. Outlet Tubing The detector’s Teflon outlet tubing can be directed three different ways: •...
  • Page 33 Installation Capillary The accessory package for the capillary flow cell includes the Ultra-Low Volume Back Pressure Regulator. The inlet tubing has an arrow pointing toward the back pressure regulator and the outlet arrow points away. Ultra-Low Volume Back Pressure Regulator 2-14 Artisan Technology Group - Quality Instrumentation ...

  • Page 34: Operation

    You can also program the detector to choose new parameters at any preset time during a run. The 155 Detector can be controlled via its front panel or via external software, such as Gilson UniPoint™ System Software. The 156 Detector must be controlled via external software since that detector does not have a front panel display.

  • Page 35: Operation Flowchart

    Operation Operation Flowchart The following page contains an operation flowchart. This flowchart can help you troubleshoot the most common detector problems. Some of the problems (for example, lamp age, coated flow cell) may not appear on a new detector. They are included so the chart remains useful over the lifetime of the detector.
  • Page 36 Operation Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 37: Front Panel Diagram

    Operation Front Panel Diagram Following is a diagram and description of the front panel for a 155 Detector. If you have a 156 Detector, your front panel only includes the LAMP ON/OFF key and the status indicators. LAMP ON/OFF Press this key to turn the UV and visible lamps on and off.
  • Page 38 Operation Soft keys Keys whose functions are determined by the software. When you advance to a new display, the soft keys may assume new functions. The current soft key function is listed on the display directly above each key. HELP Press the HELP key to show a description of the current display.

  • Page 39: Software Structure

    Operation Software Structure To operate the detector, you select the operating mode and then set the run conditions for that mode. You press soft keys to show and select options when in a mode. Mode Selection At the core of the detector software is mode selection.
  • Page 40 Operation The detector won’t let you enter an out-of-range value for a parameter. If your entry is too high or too low, the software displays a message specifying the correct range of values for the parameter. Change Use this soft key to select predefined settings for a parameter.
  • Page 41 Operation Mode The Mode soft key returns you to the Select Mode display, shown below: If you’re in the status or setup mode, press ESC to return to the first detection mode display. Then press Mode to return to the Select Mode display. If you are in the file mode you may need to press ESC several times to return to the first detection mode display.
  • Page 42 Operation Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 43 Operation 3-10 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 44 Operation 3-11 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 45: Start Up

    Operation Start Up Follow the instructions in Section 2, Installation, to make all electrical and plumbing connections. If you see an error message when starting the detector, refer to page 3-15. Wake-Up Displays Turn on the detector by pressing the rear-panel MAINS switch.
  • Page 46 Operation Next, the display shows the conditions for the last-used detection mode (single, dual, or scan wavelength). The bottom line lists soft key commands. For example, if single wavelength mode was the last mode used, you might see the following: The detector stores all of your entries in its permanent memory, so the detector always “wakes up”...

  • Page 47: Selecting The Mode

    Operation Selecting the Mode To access a different mode, press Mode. You’ll see: Then press the soft key for the mode you want to enter. You’ll see the first display for the selected mode. The soft keys identify the options available. The remainder of this section describes how to use the setup, single wavelength, dual wavelength, scan wavelength and file modes.

  • Page 48: Error Messages

    The UV lamp needs to be replaced, or there is an internal misalignment. Perform UV Lamp Maintenance described on page 4-22. Contact Gilson if the problem persists. Low Visible Energy The visible lamp is disconnected or needs to be replaced, or there is an internal misalignment.

  • Page 49: Detector Setup Parameters

    Note: If you’re using Gilson control software and collecting data via the GSIOC, the software uses the mV full scale and % offset parameters set in its dialog box(es).

  • Page 50: Second Display For Setup Mode

    Operation Second Display For Setup Mode Following is a description of the parameters on the second display for setup mode. When you’re finished checking or changing parameters, press the Next soft key to reveal the next display for setup mode. Parameter Description UV lamp alarm...

  • Page 51: Third Display For Setup Mode

    Operation Third Display For Setup Mode Following is a description of the parameters on the third display for setup mode. When you’re finished checking or changing parameters, press the Next soft key to reveal the next display for setup mode. Parameter Description Event channel(s)

  • Page 52: Fourth Display For Setup Mode

    Operation Fourth Display For Setup Mode Following is a description of the parameters on the fourth display for setup mode. When you’re finished checking or changing parameters, press Previous until you see the first display for setup mode. Parameter Description Concentration factor Set this multiplier if you want the display to show readings in units other than AU (absorbance units).

  • Page 53: Single Wavelength Mode

    Operation Single Wavelength Mode In single wavelength mode, you can monitor a sample at any wavelength from 190 to 700 nm, at 1 or 2 sensitivities. Plus, you can direct one output channel to trace the percent of UV or visible light transmitted through the sample.

  • Page 54: Sensitivity

    Operation Sensitivities 1 & 2 In single wavelength mode, the detector can monitor a sample at two sensitivities on separate output channels. Set these parameters to reflect the two sensitivities you want to display. The default sensitivity setting for output channels 1 and 2 is 0.01 AUFS.

  • Page 55: Output Channels

    Operation Output Channels The following table lists what data are transmitted via each output channel. Channel 1: detection at sensitivity 1 Channel 2: detection at sensitivity 2 Channel 3: percent transmittance Note: The output from channel 3 shows the percent of input UV or visible light that passes through the sample and reaches the active cell detector.

  • Page 56: Example Run

    Operation Example Run You can use your HPLC system to separate a mixture of herbicides. You’ll monitor the column effluent at 235 nm. And, since the components are present in low amounts, you’ll monitor at high sensitivity (0.005 AUFS). When monitoring at a single sensitivity, you only need to connect output channel 1 to your recorder.
  • Page 57 Operation Under these conditions, and at a chart speed of 1 cm/min, the herbicide trace analysis looks like this: 3-24 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 58: Dual Wavelength Mode

    Operation Dual Wavelength Mode In dual wavelength mode, you can simultaneously monitor two wavelengths. The sensitivity is set independently for each monitor wavelength. Via output channel 3, you can obtain the ratio of the signals at the two monitor wavelengths. If the display on the next page is not shown, press the Mode soft key at the first display of the currently selected detection mode.

  • Page 59: First Display For Dual Wavelength Mode

    Operation First Display for Dual Wavelength Mode Following is a description of the parameters on the first display for dual wavelength mode. The absorbances at the currently selected wavelengths appear in the first line of the display. You use the display to set new wavelengths and sensitivities for output channels 1 and 2.

  • Page 60: Second Display For Dual Wavelength Mode

    Operation Second Display for Dual Wavelength Mode Following is a description of the parameters on the second display for dual wavelength mode. To return to the first display for dual wavelength mode, press the Previous soft key. Parameter Description Peak width The detector must know the width of the narrowest peak in your run.
  • Page 61 Operation Ratio threshold In dual wavelength mode, output channel 3 shows a ratio of the absorbance at wavelength 1 to the absorbance at wavelength 2. The ratio can help you determine peak purity. The absorbance ratio is displayed only when the absorbance at both wavelengths exceeds a specified threshold.

  • Page 62: Output Channels

    Operation Output Channels The following table lists what data are transmitted via each output channel. Channel 1: detection at wavelength 1 (sensitivity 1) Channel 2: detection at wavelength 2 (sensitivity 2) Channel 3: ratio of wavelength signals Example Run You can use your HPLC system to separate a mixture of polynuclear aromatic hydrocarbons (PAH).
  • Page 63 Operation Set parameters Follow these steps to set the detection parameters: To set the first monitor wavelength (240 nm), press 240 on the keypad, and then press ENTER. To set the second monitor wavelength (287 nm), press 287 on the keypad, and then press ENTER.
  • Page 64 Operation Set the ratio threshold to 0.01, and then press ENTER. At this setting, a ratio is displayed only when the trace at both wavelengths is above 0.01 AU. Since the full-scale height at both wavelengths is 0.2 AU, a ratio appears only when peak heights on both traces are greater than 5% of full scale.

  • Page 65: Scan Wavelength Mode

    Operation Scan Wavelength Mode In scan wavelength mode, you can locate wavelengths of maximum absorbance by scanning peak material across a range of wavelengths. Monitor your sample at any wavelengths between 190 and 700 nm, at one or two sensitivities. Scan data are displayed on output channel 3.

  • Page 66: First Display For Scan Wavelength Mode

    Operation First Display for Scan Wavelength Mode Following is a description of the parameters on the first display for scan wavelength mode. The absorbance at the currently selected wavelength appears in the first line of the display. You use the display to set the new monitor wavelength, sensitivities for output channels 1 and 2, and peak width.
  • Page 67 Operation Peak width The detector must know the width of the narrowest peak on your chromatogram. The detector uses this information to optimize the presentation of peaks and to minimize baseline noise. To set the peak width accurately, run a chromatogram using the default peak width setting.

  • Page 68: Second Display For Scan Wavelength Mode

    Operation Second Display for Scan Wavelength Mode Following is a description of the parameters on the second display for scan wavelength mode. Parameter Description Sensitivity 3 Set this parameter to the sensitivity setting to be in effect during the scan. The default sensitivity setting for output is 0.010 AUFS.

  • Page 69: Third Display For Scan Wavelength Mode

    Operation Third Display for Scan Wavelength Mode Following is a description of the parameters on the third display for scan wavelength mode. Parameter Description Automatic scan initiation When automatic scan initiation is “On” and you press the Scan soft key, the scan is not performed until the absorbance reading reaches the specified limitation threshold, described below.

  • Page 70: Remote Event/Zero

    Operation Remote Event/Zero If the detector is connected to a computer or sampling injector, the scan and zero functions can be initiated remotely via the remote event (scan) and autozero (zero scan) connection. Scan Mode Event Marker In the scan wavelength mode, output channel 3 contains a special event mark function.

  • Page 71: Discrete Sample Scan

    Operation Discrete Sample Scan To scan a single sample dissolved in a buffer, follow these instructions. Locate one 1/4-28 coupler and one male Luer end-fitting from the accessory package. Make the following connections: • Attach the coupler to the detector outlet •...

  • Page 72: Example Run

    Operation Example Run You can use your HPLC system to set up conditions for monitoring pyrene. You know that you can detect a pyrene peak at 254 nm, but you want to look for other absorbance maxima between 210 nm and 340 nm.
  • Page 73 Operation Set parameters Follow these steps to set the detection parameters: To set the monitor wavelength (254 nm), press 254 on the keypad, and then press ENTER. To set the sensitivity at the monitor wavelength, press 1, and then press ENTER. Since you only want to use one sensitivity to monitor at 254 nm, disregard the parameter for the second sensitivity.
  • Page 74 Operation 10 Press Next to see additional parameters for scan wavelength mode. You’ll see: 11 Press Previous until you see the first display for the scan wavelength mode. Under these conditions, and a chart speed of 2 cm/ min, the pyrene scan looks like this. 3-41 Artisan Technology Group - Quality Instrumentation ...

  • Page 75: Programming The Detector

    Operation Programming the Detector In file mode, you can create a program file that specifies the parameters to be set each time you use the detector. This is convenient in laboratories where individuals operate the same detector under different detector conditions. File mode can also be used to vary the parameters during a run.

  • Page 76: Remote Event

    Operation Remote Event A remote event signal tells the detector to continue programmed operation. For example, you can specify a Wait for contact event in the program file. Then, you can instruct the sampling injector to send a remote signal to the detector after sample injection.

  • Page 77: Programming Tools

    Operation Programming Tools Your programming tools are the numeric keypad, the arrow keys, and the soft keys found on the file mode displays. You use the numeric keypad to enter values for parameters. You use the up and down arrow keys to view the events listing for the current file.

  • Page 78: Example 1: Startup File

    Operation Example 1: Startup File This tutorial shows you how to create a sample program file. You’ll set up a file that contains detection and setup parameters that you want to use each time you operate the detector. If you run this file before using the detector, you can be assured that the parameters you use today are the same as those used yesterday.
  • Page 79 Operation To create program file 1, press 1 on the keypad, and then press Edit. Or, if file 1 already exists, choose 0 or a number from 2 to 9. Then press Edit. After you press Edit, all of the detection and setup parameters in the detector’s memory are copied to the file.
  • Page 80 Operation Type 0.01 and press ENTER. Press Add to insert the event into the file. You’ll see: Run the file Now each time before you use the detector, run the file you created above. To do this: Access the file mode as described on page 3-42. Type the number of the file.

  • Page 81: Example 2: Programmed Run

    Operation Example 2: Programmed Run This tutorial shows you how to program the detector to: • begin a run under one set of conditions • complete the run by monitoring at different wavelength and sensitivity parameters Conditions You are monitoring a three-peak sample in single wavelength mode at: •...
  • Page 82 Operation Indicate first set of conditions using single wavelength detector mode As stated earlier, the detector automatically copies all detector parameters currently in memory to a newly created program file. Therefore, you can set up the initial run conditions using the single wavelength mode instead of the file mode.
  • Page 83 Operation Since you only want to monitor at one sensitivity, do not change the second sensitivity. You can either ignore the trace generated at Sensitivity 2 or disconnect output channel 2, which carries that trace, from the detector. At half height, the narrowest peak in the run is 10 seconds in duration.
  • Page 84 Operation Indicate user events Once you’ve selected the file number, you’ll see: In addition to the pre-stored time 0.00 events, you’ll specify events that do the following: • zero the baseline at 0.01 min • indicate a wait (for sample injection) at 1.0 min •...
  • Page 85 Operation Press Add to insert the event into the file. You’ll see the timed event listing. You can use the up and down arrow keys to scroll through the listing. Press Add to insert another event. Set the wait (for sample injection) To set the wait event: At the Select the type of event to add display, press Setup.
  • Page 86 Operation Change wavelength and sensitivity To change the wavelength and sensitivity: At the Select the type of event to add display, press Single to select the single wavelength mode. You’ll see: Press the down arrow key. You’ll see: For the minutes parameter, press 2.5 on the keypad and press ENTER.
  • Page 87 Operation Press the down arrow key until you see: For the minutes parameter, press 2.5 on the keypad and press ENTER. 10 For the sensitivity parameter, press 0.02 on the keypad and press ENTER. 11 Press Add to insert the timed event. 12 At the display showing timed events, press Add to insert another event.
  • Page 88 Operation Run the program file You can now run the program that you just wrote. Doing so will help you learn how the display presents programmed events during an actual run. At the following screen, type the number of the created file then press ENTER.

  • Page 89: Example 3: Linking To Another File

    Operation Example 3: Linking to Another File At the following display, press Setup. Press the down arrow key until you see: Type the time at which to link from one file to another and press ENTER. Type the file number that you want to execute and press ENTER.

  • Page 90: Mobile Phase Tips

    Operation Mobile Phase Tips Degas Solvents and Buffers Always use degassed, HPLC-grade solvents (including water) and buffers for your mobile phase. If the back pressure on the flow cell is sufficiently low, gas bubbles may still appear, even when using degassed solvents.
  • Page 91 Operation The table below lists commonly used solvents with low UV and visible cutoffs. Solvent UV/Visible cutoff Acetonitrile 190 nm Cyclohexane 200 nm Cyclopentane 200 nm Decahydronaphthalene 200 nm Ethanol 210 nm Heptane 200 nm Hexadecane 190 nm Hexane 195 nm Hexanes 210 nm Isooctane...

  • Page 92: Maintenance

    If these do not solve the problem, contact the Gilson Customer Service Department or your Gilson representative. Refer to the Before Calling Us information on page 5-10.

  • Page 93: Flow Cell Maintenance

    Be extremely careful when working with the flow cell and its fittings. Flow cells are considered expendable and are not covered by Gilson’s warranty if damaged or broken during any maintenance procedure. Cleaning the Inside of the Flow Cell...
  • Page 94 Maintenance Solvent cleaning If you suspect that droplets of an organic-soluble contaminant or immiscible solvent contaminate the active flow cell, draw or pump a series of miscible solvents through the cell. If you were pumping a polar mobile phase, you should draw methanol, tetrahydrofuran, methylene chloride, and then methanol through the flow cell.
  • Page 95 Maintenance Acid cleaning If you suspect that residual proteins contaminate the flow cell, draw 50% nitric acid through the cell. Acid cleaning is a more thorough technique, though much more care must be taken. CAUTION! Take all necessary precautions so that acid does not come into contact with eyes, skin, clothing and equipment surfaces.

  • Page 96: Unclogging The Flow Cell

    Maintenance Unclogging the Flow Cell To try to eliminate a blockage in the active cell or in its inlet or outlet tubing, pump solvent backwards through the flow cell. Connect a high-pressure pump to the outlet and direct the inlet to waste. For the pump, set the maximum pressure below 500 psi (34 bar).
  • Page 97 Maintenance Analytical or preparative flow cell To access and remove the flow cell assembly: Open the detector’s front door. Using a 5/32" Allen wrench, remove the two screws on the front of the detector block and move the block to the side. Using a Phillips screwdriver, remove the flow cell assembly screw (refer to diagram below for location of the screw).
  • Page 98 Maintenance To remove flow cell: Loosen the fittings for the inlet and outlet tubing. The inlet tubing enters the flow cell assembly from the bottom while the outlet tubing exits from the top. Using a 1/16" Allen wrench, loosen the stainless steel screw located on the left side of the flow cell assembly.
  • Page 99 Maintenance To replace the inlet tubing: When replacing the inlet tubing, ensure that its ID is appropriate for the flow cell (analytical or preparative). See Appendix E for a list of replacement parts. Remove the inlet tubing clamp and set it aside. Unscrew the male nut that connects the inlet tubing to the flow cell assembly.
  • Page 100 Maintenance Press together the two segments of inlet tubing as shown in the diagrams below. The segment leading away from the flow cell should be almost in front of the segment leading into the flow cell. Insert the inlet tubing clamp into its socket and tighten.
  • Page 101 Maintenance To clean and insert flow cell: To clean the existing or replacement flow cell before installing it, dampen the quartz windows with alcohol or a laboratory cleaning solution. Then wipe the windows with a piece of lens paper or lint-free towel. Clean the inside of the flow cell mounting area with a lint-free towel soaked in alcohol.
  • Page 102 Maintenance To check for leaks: To determine whether the fittings are leak-free, use a syringe to initiate flow through the cell. Check carefully along the sides of the cell for beads of liquid. A flashlight may be helpful. If leakage is detected visually or if the area around the fitting feels cool to the touch, remove and clean the flow cell as well as its chamber.
  • Page 103 Maintenance Microbore flow cell To access and remove the flow cell assembly: Open the detector’s front door. Using a 5/32" Allen wrench, remove the two screws on the front of the detector block and move the block to the side. Using a Phillips screwdriver, remove the flow cell assembly screw (refer to diagram below for location of the screw).
  • Page 104 Maintenance To remove the flow cell: Loosen the fittings for the inlet and outlet tubing. The inlet tubing enters the flow cell assembly from the bottom while the outlet tubing exits from the top. Using a 1/16" Allen wrench, loosen the stainless steel screw located on the left side of the flow cell assembly.
  • Page 105 Maintenance To clean and insert the flow cell: To clean the existing or replacement flow cell before installing it, dampen the quartz windows with alcohol or a laboratory cleaning solution. Then wipe the windows with a piece of lens paper or lint-free towel. Clean the inside of the flow cell mounting area with a lint-free towel soaked in alcohol.
  • Page 106 Maintenance To check for leaks: To determine whether the fittings are leak-free, use a syringe to initiate flow through the cell. Check carefully at the tubing connections to the flow cell for beads of liquid. If you notice leakage, carefully tighten the fittings and dry all surfaces.
  • Page 107 Maintenance SFC or preparative SFC flow cell To replace the flow cell window and other components for the SFC flow cell, order the SFC rebuild kit (part number 10043888). Instructions for rebuilding the flow cell are supplied with the kit. To access and remove the flow cell assembly: Open the detector’s front door.
  • Page 108 Maintenance Refer to the following diagrams when replacing the flow cell and/or tubing. Flow cell assembly, assembled Flow cell assembly, disassembled To replace the outlet tubing: When replacing the outlet tubing, ensure that its ID is appropriate for the SFC flow cell. See Appendix E for a list of replacement parts.
  • Page 109 Maintenance To replace the inlet tubing: When replacing the inlet tubing, ensure that its ID is appropriate for the SFC flow cell. See Appendix E for a list of replacement parts. If necessary, refer to the flow cell diagrams on page 4-17 when replacing the inlet tubing as described below.
  • Page 110 Maintenance Press together the two segments of inlet tubing as shown in the diagrams below. The segment leading away from the flow cell should be almost in front of the segment leading into the flow cell. Insert the inlet tubing clamp into its socket and tighten.
  • Page 111 Maintenance To check for leaks: To determine whether the fittings are leak-free, use a syringe to initiate flow through the cell. Check carefully at the tubing connections to the flow cell for beads of liquid. If you notice leakage, carefully tighten the fittings and dry all surfaces. To replace the flow cell assembly, replace the detector block, and close the detector door: Insert the flow cell assembly into the detector...
  • Page 112 Maintenance Capillary flow cell To access and remove the flow cell assembly: CAUTION! The inlet and outlet tubing on the capillary flow cell are fragile. Be careful when opening and closing the front door of the detector and removing the cell. If broken, this tubing cannot be replaced.

  • Page 113: Lamp Maintenance

    Maintenance Lamp Maintenance The detector contains a deuterium lamp for monitoring UV wavelengths and a tungsten/ halogen lamp for monitoring visible wavelengths. The UV lamp has a warranted life of 750 hours or 180 days. The visible lamp has a 500-hour warranted life.
  • Page 114 Maintenance Disconnect visible lamp connector and remove lamp Locate the visible lamp. Follow the visible lamp’s wires to locate the connector that links the wires to the internal circuit board. Disconnect the connector from the internal circuit board. Grasp the visible lamp and turn it until the flat edge faces upward.
  • Page 115 Maintenance Remove lamp housing and disconnect UV lamp connector Loosen the three thumbscrews that secure the lamp housing to the monochromator casting. While loosening the last thumbscrew with your right hand, support the lamp housing with your left hand. Bring the lamp housing towards you. Follow the UV lamp’s wires to locate the connector that links the wires to the internal circuit board.
  • Page 116 Press LAMP ON/OFF. If the lamp fails again, there may be an internal alignment, a power supply, or a starting circuitry problem. Contact the Gilson Customer Service Department or your Gilson representative. See the Before Calling Us information on page 5-10. 4-25...
  • Page 117 See Appendix D for a listing of GSIOC commands. To reset the lamp hours via the front panel of a 155 Detector: At the display, press Mode. You’ll see: Press Status to access status mode. Press Next until you see: Press NewUV to set the lamp hours to 0.
  • Page 118 Or, the software should allow you to send a GSIOC command to set the lamp alarm. See Appendix D for a listing of GSIOC commands. To set the lamp alarm via the front panel of a 155 Detector: Press Mode. Press Setup to access setup mode.
  • Page 119 Do not turn the lamps off. Reset the lamp alarm. To reset the lamp alarm for the 156 Detector, refer to the user’s guide for the Gilson control software. The software should include a command that resets the lamp alarm. Or, the software should allow you to send a GSIOC command to reset the lamp alarm.

  • Page 120: Visible Lamp Maintenance

    Maintenance Visible Lamp Maintenance CAUTION! Never touch a hot lamp. Always wait 30 minutes or more after turning the lamp off before replacing the lamp What you’ll need • Replacement lamp • Flashlight Get detector ready for lamp maintenance Press LAMP ON/OFF. Turn off the rear-panel MAINS switch.
  • Page 121 Maintenance Remove visible lamp Locate the visible lamp. Follow the visible lamp’s wires to locate the connector that links the wires to the internal circuit board. Disconnect the connector from the internal circuit board. Note: If the connector was not secure in its socket, you may want to secure the connector and start the detector to determine if the loose connector caused the problem.
  • Page 122 Turn on MAINS switch. Press LAMP ON/OFF. If the lamp fails again, there may be an internal alignment, a power supply, or a starting circuitry problem. Contact your local representative or Gilson. See the Before Calling Us information on page 5-10. 4-31...
  • Page 123 See Appendix D for a listing of GSIOC commands. To reset the lamp hours via the front panel of a 155 Detector: At the display, press Mode. You’ll see: Press Status to access status mode. Press Next until you see: Press NewVis to set the lamp hours to 0.
  • Page 124 Or, the software should allow you to send a GSIOC command to set the lamp alarm. See Appendix D for a listing of GSIOC commands. To set the lamp alarm via the front panel of a 155 Detector: Press Mode. Press Setup to access setup mode.
  • Page 125 To reset the lamp alarm for the 156 Detector, refer to the user’s guide for the Gilson control software. The software should include a command that resets the lamp alarm. Or, the software should allow you to send a GSIOC command to reset the lamp alarm.

  • Page 126: Fuse Replacement

    A blown fuse may indicate the existence of another problem in the instrument. If the replacement fuses blow, don’t try others. Contact your local representative or Gilson. Refer to the Before Calling Us information on page 5-10. 4-35 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 127 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 128: Troubleshooting

    • diagnostic techniques you can use with Gilson service personnel to troubleshoot problems with the detector’s lamp and optics • information about how and when to contact the Gilson Customer Service Department or your Gilson representative about repairs Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 129: Detector Not Functioning

    • Check cord and power connection. • Fuses may be blown. Refer to Fuse Replacement on page 4-35. If the problem persists, contact the Gilson Customer Service Department (refer to page 5-10 for contact information) or contact your Gilson representative.

  • Page 130: Baseline Spikes

    Troubleshooting Baseline Spikes • Be sure solvents are degassed. • Check fittings for a leak in system. Repair as needed. • Reduce pump noise by changing the compressibility setting on the pump and by examining check valves. • Voltage transients on a single circuit can interfere with detector output.

  • Page 131: Baseline Noise

    Troubleshooting Baseline Noise • Allow each lamp to warm up for at least 1 hour. • Eliminate drafty air currents and variations in ambient temperature. Move the detector away from windows or doors. • Eliminate smoke from the environment. • Check grounds on all instruments. Eliminate ground loops by connecting the detector and recorder to the same power outlet.

  • Page 132: Baseline Drift

    Troubleshooting Baseline Drift • Allow each lamp to warm up for at least 1 hour. • Eliminate changes in ambient temperature. If drift is dependent on temperature, eliminate drafts and avoid areas of direct sunlight. • Check for contaminated or “bleeding” column. If drift disappears after removing column connections, regenerate or replace column.

  • Page 133: Autozero Out Of Range

    Troubleshooting Autozero Out of Range This message results from high background absorbance. The detector cannot reduce the baseline to zero, but will reduce the baseline as much as possible. Operation continues during and after you receive this message. • Flow cell may be coated with highly absorbing eluents.

  • Page 134: Peaks Too Broad

    Lamp Maintenance on page 4-22. If none of the above fix the problem, contact the Gilson Customer Service Department (refer to page 5-10 for contact information) or your Gilson representative. Peaks Too Broad • Check peak width setting - it may be set too high.

  • Page 135: Diagnostics

    That current is proportional to the intensity of the light. Numeric Analyses on the 155 Detector The Gilson service personnel can gain insight into detector malfunction by examining voltage percentages at various wavelengths. To provide this information to Gilson, do the following: Ensure that the flow cell is dry or contains only HPLC-grade water.
  • Page 136 Troubleshooting Press Next until you see a display like the following: Type 190 for the wavelength and press ENTER. Wait until the AU reading stabilizes. In tabular form, record the displayed AU, Active, and Reference values. For the Active % and Reference %, values up to 110% are within normal operating parameters for the detector.

  • Page 137: Repair And Return Policies

    Troubleshooting Repair and Return Policies Telephone Numbers In the United States, Gilson Customer Service can be reached by calling 800-445-7661 or 608-836-1551. Outside the United States, contact your Gilson representative. Before Calling Us Gilson Customer Service personnel will be able to...

  • Page 138: Rebuilt Exchange

    For some Gilson devices, rebuilt exchange components are available. Contact Gilson Customer Service for details. Return Procedure In the United States, contact the Gilson Customer Service Department to obtain authorization before returning any Gilson equipment. To return a piece of equipment: Carefully pack the detector to prevent damage •...
  • Page 139 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 140: Setup Mode

    Defaults and Limits Note: When you first use your new detector, default conditions and values are applied until modified. Setup Mode Parameter Default High Unit Voltage scales 1000 Channel offsets 1000 Vis lamp alarm 9999 hours UV lamp alarm 9999 hours Event channels Autorange channels...

  • Page 141: Dual Wavelength Mode

    Appendix Dual Wavelength Mode Parameter Default High Unit Wavelength 1 Wavelength 2 Sensitivity 1 0.010 0.001 2.000 AUFS Sensitivity 2 0.010 0.001 2.000 AUFS Peak width 12.0 99.0 Ratio multiplier 1.00 0.01 99.99 Ratio threshold 0.00100 0.00001 2.00000 Scan Mode Parameter Default High...

  • Page 142: Mode-Specific Output Channels

    Mode-Specific Functions Mode-Specific Output Channels Mode Channel 1 Channel 2 Channel 3 Single wavelength 1 at sensitivity 1 wavelength 1 at sensitivity 2 % transmittance Dual wavelength 1 at sensitivity 1 wavelength 2 at sensitivity 2 ratio Scan monitor wavelength at sensitivity 1 monitor wavelength at sensitivity 2 scan at sensitivity 3 Mode-Specific Remote Event and Autozero Functions...
  • Page 143 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 144: Sensitivity

    Sensitivity To set the sensitivity, you must consider the sample concentration. You can ensure that your peaks appear on-scale by running test chromatograms at various SENSITIVITY settings. When you set the SENSITIVITY to a small number, the detector will monitor at high sensitivity.
  • Page 145 Appendix At a constant SENSITIVITY setting, the peak height varies as the sample concentration changes. • At the same SENSITIVITY setting, a sample with an absorbance of greater than 1.0 produces a peak height that is greater than full scale. •...
  • Page 146 Appendix At a constant sample concentration, the peak height varies as the SENSITIVITY setting changes. • At a SENSITIVITY setting of 1.0 AUFS, a sample with an absorbance of 0.1 AU produces a maximum peak height that is less than full scale. •...
  • Page 147 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 148: Gsioc Control

    GSIOC Control The Gilson Serial Input/Output Channel (GSIOC) is an asynchronous serial communications interface that enhances the power of Gilson devices, such as a 155 or 156 Detector. Communication occurs via the GSIOC or RS-232 connection between the system controller and detector.

  • Page 149: Gsioc Commands

    Appendix GSIOC Commands There are two kinds of commands that you can issue from the system controller to the detector. • Buffered commands send instructions to the detector. These commands are executed one at a time. • Immediate commands request status information from the detector.
  • Page 150 Appendix Command Type Description Identifies the detector. Returns a character string that identifies the model number and software version for the detector, for example: “155V1.00” Determines if the first display for single, dual, or scan wavelength mode is shown. If the first display is shown, returns “T”...
  • Page 151 Appendix Pauses the currently executing file. Resumes the currently paused file. Identifies the editable field that has the focus. If the focus is at an editable field, returns “b,e,c” where: b - Index of the beginning character of the editable field e - Index of the last character of the editable field c - Index of the cursor The index is a number from 0 to 159 that identifies a location...
  • Page 152 Appendix K=xx...x Simulates front panel key presses. Keystrokes are simulated according to the key assignments shown in the diagram below. For example, if you wanted to simulate the pressing of the HELP key, you would use the following command: K=H To lock the keypad without sending any keystrokes, send the following command: K= To unlock the keypad so you can use it to specify parameters,...
  • Page 153 Appendix Sets the UV lamp hours to 0 (zero). Sets the visible lamp hours to 0 (zero). If both lamps are lit, returns “uuuu vvvv” where: uuuu - UV lamp hours vvvv - Visible lamp hours Returns “Min=xxx Max=yyy” where: xxx - Wavelength at which the minimum absorbance was obtained during the last scan.
  • Page 154 Appendix Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 155 Appendix Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 156 Appendix Reads reference signal current. Returns: “n..n” in µFS units. Wn=xx.xx Disconnects and writes to the display. Or, reconnects the display after it was disconnected. When specifying parameters for the command: - Line number (0 to n–1, n being the line number). For instance, if you’re writing to line 1, indicate 0 for n.
  • Page 157 Appendix Identifies the contents of the front panel display. Returns “Wn=xx..xx” where: - Display line number minus 1. xx...xx - Up to a 40-character alphanumeric string written to the display using the buffered W command. Note: The first line that is returned is the last defined by the buffered W command.

  • Page 158: Fifo Command List

    Appendix FIFO Command List The compressed digital data from every input and output channel can be read by the master device. To determine what data is present on each channel, consult the mode descriptions in Operation. I=Immediate B=Buffered Command Type Description 0xxxx Flushes FIFO 0 (Output channel 1 data).
  • Page 159 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 160: Replacement Parts

    Replacement Parts Lamp Assemblies 100326 Deuterium Lamp Assembly for 15X-series (UV wavelengths). Warranted 750 hours or 180 days. 100325 Tungsten/halogen Lamp Assembly for 15X-series (VIS wavelengths) 1500 hour life Cell/Accessory Kits 104445 Analytical flow cell/accessory kit (5 mm pathlength, 12 µL volume, quartz) with stainless steel inlet tubing 104445LP Low pressure flow cell/accessory kit (5 mm pathlength, 12 µL volume, quartz) with stainless steel inlet tubing...

  • Page 161: Flow Cell Assemblies

    Appendix 1044395 Preparative SFC flow cell/accessory kit (0.5 mm pathlength, 2 µL volume, stainless steel and quartz) with stainless steel inlet and outlet tubing 104446 Capillary flow cell/accessory kit (8 mm pathlength, 35 nL volume) glass capillary inlet and outlet tubing. Flow Cell Assemblies 100405 Analytical flow cell (5 mm pathlength, 12 µL volume,...
  • Page 162 Appendix 10043851 SFC inlet tubing, formed 0.005" ID stainless steel; no fittings, use Upchurch U-400 male nut and LT-100 ferrule to make connection to flow cell 1007455 Analytical outlet tubing, 0.3 mm Teflon, with omnifit fittings 1007415 Preparative outlet tubing, 0.8 mm Teflon, with omnifit fittings 1007425 Microbore outlet tubing, 0.006"...

  • Page 163: Miscellaneous

    Appendix Miscellaneous 36070905 Back pressure regulator (75 psi), PEEK 36070906 Back pressure regulator (75 psi), stainless steel 4311562 Allen wrench, 5/32", for detector block mounting screws 4310621 Allen wrench, 1/16", for stainless steel screw on left side of flow cell assembly 10093872 Torque wrench for SFC flow cell assembly, 40 in.-lbs.

  • Page 164: Display Adjustment

    Display Adjustment You can use the Display View Angle Adjustment feature to improve the readability of text on the detector’s display. Do one of the following: a) If the detector is not turned on, press the rear-panel MAINS switch. b) If the detector is turned on and the lamps are lit, press LAMP ON/OFF. Wait until there is no text on the display.
  • Page 165 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

This manual is also suitable for:

156

Table of Contents