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Agilent Technologies 1100 Series Reference Manual

Fluorescence detector
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  • Page 1 Agilent 1100 Series Fluorescence Detector Reference Manual...
  • Page 2 Agilent to establish implied, with regard to this manual acceptable terms in a written agreement and any information contained © Agilent Technologies, Inc. 1998, 1999- executed by all relevant parties. herein, including but not limited to 2004...
  • Page 3 How to start with the detector Optimizing the Fluorescence Detector Detection with the Agilent 1100 series fluorescence detector, either fluorescence or phosphorescence, can give you very sensitive and selective results if you understand what you are doing and why. This chapter explains in detail how to optimize detection.
  • Page 4 This chapter is intended to introduce an operator to the screens available for operation of the Agilent 1100 diode array detector with the Agilent 1100 control module. Please use the manual of Control module for further detailed reference. Specifications Performance specifications of the detector 1100 Series FD Reference Manual...

  • Page 5: Table Of Contents

    Observe the maxima via the isoabsorbance plot Method Development Step 1: Check the LC system for impurities Step 2: Optimize limits of detection and selectivity Step 3: Set up routine methods Example: Optimization for Multiple Compounds 1100 Series FD Reference Manual 5...
  • Page 6 O er ie of the Dete tor’s I di ators a d Test Fu tio s Status Indicators Power Supply Indicator Detector Status Indicator Error Messages Time-out Shutdown Remote Time-out Synchronization Lost Leak Leak Sensor Open 1100 Series FD Reference Manual...
  • Page 7 Wavelength Verification and Calibration Check of Raman Band of Water The Wavelength Calibration Procedure Preparation of the Glycogen Calibration Sample Preparation of the Flow Cell Wavelength Calibration Verification Test Functions Lamp Intensity Test Lamp Intensity History 1100 Series FD Reference Manual 7...
  • Page 8 Exchanging Internal Parts Removing the Covers Removing the Rear Foam Exchanging the Lamp Exchanging the EX-condenser Replacing the Lamp Cover Window Exchanging the Processor Board Exchanging the Fan Exchanging the Leak Sensor or Leak Panel 1100 Series FD Reference Manual...
  • Page 9 Replacing the Interface Board Repla i g the Dete tor’s Fir 6 Identifying Parts and Materials Overview of Main Assemblies Optical Unit Assembly Lamp Cover Parts Control Module Sheet Metal Kit Plastic Parts Foam Parts 1100 Series FD Reference Manual 9...
  • Page 10 CAN Cable External Contact Cable RS-232 Cable Kit LAN Cables Introduction to the Fluorescence Detector Introduction to the Detector How the Detector Operates Raman Effect Optical Unit Reference System Analytical Information From Primary Data Fluorescence Detection 1100 Series FD Reference Manual...
  • Page 11 Firmware Description Firmware Updates Raw Data Conversion to Fluorescence (LU) Units Data flow for chromatographic output Data flow for spectral output Spectra Acquisition Modes Optional Interface Boards BCD Board LAN Communication Interface Board Interfaces 1100 Series FD Reference Manual 11...
  • Page 12 Major keys on the Agilent 1100 Control Module Screens available from the Analysis screen Screens available from the System screen Screens available from the Records screen Diagnostics and Tests Specifications Performance Specifications Safety Information General Safety Information Lithium Batteries Information 1100 Series FD Reference Manual...
  • Page 13 Radio Interference Sound Emission UV-Radiation (UV-lamps only) Solvent Information Agilent Technologies on Internet Index 1100 Series FD Reference Manual 13...

  • Page 14: Installing The Fluorescence Detector

    1100 Series FD Reference Manual Agilent 1100 Series Fluorescence Detector Reference Manual Installing the Fluorescence Detector Site Requirements Physical Specifications Unpacking the Detector Optimizing the Stack Configuration Installing the Detector Flow Connections to the Detector...
  • Page 15 Agilent Technologies Site Requirements A suitable environment is important to ensure optimal performance of the detector. Power Consideration The detector power supply has wide ranging capabilities and accepts any line voltage in the range mentioned in Table 1 on page 16. Consequently, there is no voltage selector in the rear of the detector.
  • Page 16 8 cm (3.1 inches) in the rear for air circulation and electric connections. If the bench should carry a Agilent 1100 Series system, make sure that the bench is designed to bear the weight of all modules.

  • Page 17: Physical Specifications

    ° ° Operating altitude Up to 2000 m (6500 ft) Non-operating altitude Up to 4600 m (14950 ft) For storing the detector Safety standards: IEC, CSA, UL, EN Installation category II, pollution degree 2 1100 Series FD Reference Manual 17...

  • Page 18: Unpacking The Detector

    Please report missing or damaged parts to your local Agilent Technologies sales and service office. Table 2 Detector Checklist Description Quantity Detector Power cable CAN cable (Part number 5181-1519) Flow cell 1 (built-in ) Optional flow cell/cuvette as ordered Reference Manual 1100 Series FD Reference Manual...

  • Page 19: Detector Accessory Kit Contents

    Screwdriver hexagonal 2.5 mm, 100 mm long 5965-0028 Needle-Syringe 9301-0407 Glass-Syringe 9301-1446 Calibration Sample, Glycogen 5063-6597 Sample filter, diameter=3 mm, pore size 0.45 µm 5061-3367 ( pack of 100) Wrench open end 1/4 – 5/16 inch 8710-0510 1100 Series FD Reference Manual 19...

  • Page 20: Optimizing The Stack Configuration

    Inlet Capillary (Col umn-Detector) Parts Optimizing the Stack Configuration If your detector is part of a complete Agilent 1100 Series system, you can ensure optimum performance by installing the following configuration. This configuration optimizes the system flow path, ensuring minimum delay volume.
  • Page 21 Installing the Fluorescence Detector Solvent cabinet Vacuum degasser Pump Control module Autosampler Column compartment Detector Figure 3 Recommended Stack Configuration (Front View) 1100 Series FD Reference Manual 21...
  • Page 22 Installing the Fluorescence Detector Figure 4 Recommended Stack Configuration (Rear View) 1100 Series FD Reference Manual...

  • Page 23: Installing The Detector

    3 Ensure the line power switch at the front of the detector is OFF. with green light Figure 5 Front View of Detector 4 Connect the power cable to the power connector at the rear of the detector. 1100 Series FD Reference Manual 23...
  • Page 24 NOTE 7 Connect the analog cable(s) (optional). 8 Connect the APG remote cable (optional) for non-Agilent 1100 Series instruments. 9 Turn on power by pushing the button at the lower left hand side of the detector. The status LED should be green.
  • Page 25 The detector was shipped with default configuration settings. To change these settings NOTE Setti g the - it Co figuratio S it h on page 292. 1100 Series FD Reference Manual 25...

  • Page 26: Flow Connections To The Detector

    The flow cell is shipped with a filling of isopropanol (also recommended when the NOTE instrument and/or flow cell is shipped to another location). This is to avoid breakage due to subambient conditions. 1100 Series FD Reference Manual...
  • Page 27 Installing the Fluorescence Detector 3 Assemble the column detector capillary from the 4 Assemble the waste tubing from the accessory kit. accessory kit. One side is already factory- assembled. Pre-assembled 1100 Series FD Reference Manual 27...
  • Page 28 - connecting the last detector (without column and FLD) and measuring the system pressure with flow. - the difference in measured pressure is due to the back pressure generated by the last detector and is the pressure seen by the FLD. 1100 Series FD Reference Manual...
  • Page 29 The detector should be operated with the front cover in place to protect the flow cell NOTE Establish flow and observe 8 Replace the front cover. if leaks occur. area against strong drafts from the ouside. 1100 Series FD Reference Manual 29...
  • Page 30 Installing the Fluorescence Detector 1100 Series FD Reference Manual...

  • Page 31: First Steps With The Fluorescence Detector

    Agilent 1100 Series Fluorescence Detector Reference Manual First Steps with the Fluorescence Detector Before You Start Optimization Overview Getting Started and Checkout Method Development Example: Optimization for Multiple Compounds...

  • Page 32: Before You Start

    (lower signal-to-noise ratio) when impurities are in the solvents. Flush your solvent delivery system for at least 15 minutes before checking sensitivity. If your pump has multiple channels, you should also flush the channels not in use. 1100 Series FD Reference Manual...

  • Page 33: Optimization Overview

    Selecting reference spectra at the baseline is not useful because the spectrum on the baseline is very noisy (no light!). 5 Switching lamp on only for analysis 1100 Series FD Reference Manual 33...

  • Page 34: Getting Started And Checkout

    (FLD=20 nm) which cause a systematic wavelength maximum shift depending on the absorbance spectrum of the compound under evaluation. Getting Started and Checkout This chapter describes the check out of the Agilent 1100 series fluorescence detector using the Agilent isocratic checkout sample. When required...

  • Page 35: Starting Your Detector

    Stop time 4 minutes Injection volume 5 µl Oven temperature (1100) 30 °C FLD Excitations/Emission Wavelength EX = 246 nm, EM = 317 nm FLD PMT Gain PMT = 10 FLD Response time 4 seconds 1100 Series FD Reference Manual 35...

  • Page 36: Observe The Maxima Via The Isoabsorbance Plot

    Biphenyl peak with differ ent excitation wavelengths 5 The excitation maxima is around 250 nm. Observe the maxima via the isoabsorbance plot =246 nm, λ 1 Load the data file (λ =317 nm) and open the isoabsorbance plot. 1100 Series FD Reference Manual...

  • Page 37: Method Development

    Fluorescence detectors are used in liquid chromatography when superior limits of detection and selectivity are required. Thorough method development, including spectra acquisition, is fundamental to achieve good results. This chapter describes three different steps that can be taken with the Agilent 1100 Series fluorescence detector. Table 5 gives an overview of how to benefit from the operation modes during these steps.

  • Page 38: Step 1: Check The Lc System For Impurities

    280 nm, the second-order Raleigh stray light starts above 560 nm. Stray light acts in the same way as impurities in that it simulates background noise. In both cases, a higher noise level and therefore a higher limit of detection are obtained. 1100 Series FD Reference Manual...

  • Page 39: Step 2: Optimize Limits Of Detection And Selectivity

    40) for each compound. Since this is a tedious procedure, it is applicable only when there is a limited number of compounds of interest. The Agilent 1100 Series LC offers three different ways to obtain complete information on a compound's fluorescence: Procedure I - Take a fluorescence scan offline for a single compound as described above for the mobile phase.
  • Page 40 First Steps with the Fluorescence Detector Procedure II - Use two LC runs with the Agilent 1100 Series FLD to separate the compound mix under known conditions and acquire emission and excitation spectra separately. Procedure III - Use an Agilent 1100 Series FLD/DAD combination and acquire UV/Visible spectra (equivalent to excitation spectra) with the DAD and emission spectra with the FLD-both in a single run.
  • Page 41 First Steps with the Fluorescence Detector 2 straylight 1. order 350 nm Ex 315 nm Ex 250 nm Ex Ex axis Em axis Figure 12 Characterization of a pure compound from a fluorescence scan 1100 Series FD Reference Manual 41...
  • Page 42 Excitation at 260 nm is most appropriate for all PNAs. Table 7 Conditions for Figure 13 Figure 14 on page 47 Column µ Vydac, 2.1 x 200 mm, PNA, 5 Mobile phase A = water; B = acetonitrile (50:50) 1100 Series FD Reference Manual...
  • Page 43 Injection volume µ FLD settings PMT 12, response time 4 s, step size 5 nm This shows the isofluorescence plot of emission spectra for 15 PNAs (5 µg/ml) with a fixed excitation wavelengths (260 nm). 1100 Series FD Reference Manual 43...
  • Page 44 First Steps with the Fluorescence Detector Figure 13 Optimization of the time-program for the emission wavelength 1100 Series FD Reference Manual...
  • Page 45 Timetable for the analysis of 15 polynuclear aromatic hydrocarbons Time [min] Exitation Wavelength [nm] Emission Wavelength [nm] 19.0 This timetable gives the conditions for optimum detection based on the results of two chromatographic runs. 1100 Series FD Reference Manual 45...
  • Page 46 First Steps with the Fluorescence Detector Procedure III - Make a single run with the Agilent 1100 Series DAD/FLD combination For most organic compounds, UV-spectra from diode array detectors are nearly identical to fluorescence excitation spectra. Spectral differences are caused by specific detector characteristics such as spectral resolution or light sources.
  • Page 47 First Steps with the Fluorescence Detector 2 Figure 15 spectrum and fluorescence spectra for 2,3- diaminophenazine (DAP) 1100 Series FD Reference Manual 47...

  • Page 48: Gradient

    Zorbax SB, 2 x 50 mm, PNA, 5 µm Mobile phase A = water; B = acetonitrile Gradient 0 minutes, 5% 10 minutes, 15% Flow rate 0.4 ml/min Column temperature ° Injection volume 5 µl 1100 Series FD Reference Manual...

  • Page 49: Step 3: Set Up Routine Methods

    With difficult matrices, simultaneous multi-wavelength detection offers more reliability than timetable-controlled wavelength switching. The Agilent 1100 Series FLD can, in addition, acquire fluorescence spectra while it records the detector signals for quantitative analysis. Therefore qualitative data are available for peak confirmation and purity checks in routine analysis.
  • Page 50 Very often this happens with complex matrices, influencing the retention of compounds. In spectral mode, the Agilent 1100 Series FLD can acquire up to four different signals simultaneously. All of them can be used for quantitative analysis. Apart from complex matrices, this is advantageous when watching for impurities at additional wavelengths.
  • Page 51 A match factor of 1,000 means identical spectra. In addition, the purity of a peak can be investigated by comparing spectra obtained within a single peak. When a peak is calculated to be within the user-defined purity 1100 Series FD Reference Manual 51...
  • Page 52 10.000 10.353 2.15360e-1 Fluoranthene@em 10.439 10.400 10.988 8.00754e-2 1000 Pyrene@em 12.826 12.800 13.469 1.40764e-1 Benz(a)anthracene@em 13.340 13.300 14.022 1.14082e-1 Chrysene@em 15.274 15.200 16.052 6.90434e-1 Benzo(b)fluoranthene@em 16.187 16.200 17.052 5.61791e-1 Benzo(k)fluoranthene@em 16.865 16.900 17.804 5.58070e-1 Benz(a)pyrene@em 1100 Series FD Reference Manual...

  • Page 53: Example: Optimization For Multiple Compounds

    Vydac-C18-PNA, 250 mm x 2.1 mm i.d. with 5 µm particles Sample PAH 0.5 ng Flow rate 0.4 ml/min Compressibility A (water) Compressibility B (Acetonitrile) Stroke A and B auto Time Table at 0 minutes %B=50 at 3 minutes %B=60 1100 Series FD Reference Manual 53...
  • Page 54 Figure 18 Detector Settings for Emission Scan 2 Wait until the baseline stabilizes. Complete the run. 3 Load the signal. (In this example just the time range of 13 minutes is 1100 Series FD Reference Manual...

  • Page 55: First Steps With The Fluorescence Detector 2

    First Steps with the Fluorescence Detector 2 displayed). Figure 19 Chromatogram from Emissions Scan 4 Use the isoabsorbance plot and evaluate the optimal emission wavelengths, shown in the table below. Figure 20 Isoabsorbance Plot from Emission Scan Table 13 1100 Series FD Reference Manual 55...
  • Page 56 (B, C, D). Doing so will increase the scan time and will lower the performance Figure 21 Detector Settings for Excitation Scan 6 Wait until the baseline stabilizes. Start the run. 7 Load the signal. 1100 Series FD Reference Manual...
  • Page 57 13 minutes ). Figure 23 Isoabsorbance Plot - Excitation The table below shows the complete information about emission (from Figure 20 page 57) and excitation maxima. Table 14 1100 Series FD Reference Manual 57...
  • Page 58 220 / 280 nm 7.3 min 330 nm 225 / 285 nm 7.7 min 310 nm 265 nm 8.5 min 360 nm 245 nm 10.7 min 445 nm 280 nm 11.3 min 385 nm 270 / 330 nm 1100 Series FD Reference Manual...
  • Page 59 The scan time will increase when the range is enlarged. With the default values, the scan takes about 2 minutes. NOTE 3 Set PMT gain to 16. The wavelength range and step number defines the duration. Using the maximum range, the scan would take approximately 10 minutes 1100 Series FD Reference Manual 59...
  • Page 60 A low background will improve the signal-to-noise, see also NOTE page 74. Raleigh scattering Note: This white area is normally dark blue. Raman scattering of water 2 nd order of cutoff Figure 25 Fluorescence Scan of Water 1100 Series FD Reference Manual...

  • Page 61: Optimizing The Fluorescence Detector

    Agilent 1100 Series Fluorescence Detector Reference Manual Optimizing the Fluorescence Detector Optimization Overview Design Features Help Optimization Finding the Best Wavelengths Finding the Best Signal Amplification Changing the Xenon Flash Lamp Frequency Selecting the Best Response Time Reducing Stray Light...

  • Page 62: Optimization Overview

    Optimizing the Fluorescence Detector Agilent Technologies Optimization Overview “Optimization Overview” Refer to on page 33 for details. 1100 Series FD Reference Manual...

  • Page 63: Design Features Help Optimization

    As most organic molecules absorb best in the ultra-violet range the Agilent 1100 fluorescence detector was designed to give an optimum signal-to-noise 1100 Series FD Reference Manual 63...

  • Page 64: A Real Example

    When comparing fluorescence excitation spectra directly with DAD spectra or NOTE literature based absorbance spectra, you should consider large differences in the used 1100 Series FD Reference Manual...

  • Page 65: Finding The Best Signal Amplification

    PMTGAIN was gradually raised from 4 up to 11 (the peak is from the Agilent Technologies isocratic sample which was diluted 1000 times). With increasing PMTGAIN there was an improvement in signal-to-noise up to 10. Above 10 the noise increased proportionately to the signal with no improvement in signal-to-noise.
  • Page 66 Optimizing the Fluorescence Detector Use the PMT test to automatically determine the setting. 1100 Series FD Reference Manual...

  • Page 67: Changing The Xenon Flash Lamp Frequency

    Best sensitivity can be expected with “no economy”, see Figure Standard=296 Hz Economy=74 Hz Figure 28 Xenon Flash Lamp Frequency Lamp life savings There are three ways to save lamp life: • switch to “lamp on during run” without loss of sensitivity. 1100 Series FD Reference Manual 67...
  • Page 68 Optimizing the Fluorescence Detector • switch to “economy” mode with a certain loss of sensitivity. • a combination of the above. 1100 Series FD Reference Manual...

  • Page 69: Selecting The Best Response Time

    4 seconds (default) is equivalent to a time constant of 1.8 seconds and appropriate for standard chromatographic conditions. Responsetime 2 sec Responsetime 8 sec Figure 30 Separation of Peaks using Responsetime 1100 Series FD Reference Manual 69...

  • Page 70: Reducing Stray Light

    280 nm. Because of a known set of applications a 295 nm cut-off filter is built-in for undisturbed application up to 560 nm without compromises (see Figure 31 on page 75). 1100 Series FD Reference Manual...
  • Page 71 Optimizing the Fluorescence Detector 1100 Series FD Reference Manual 71...
  • Page 72 Optimizing the Fluorescence Detector 1100 Series FD Reference Manual...

  • Page 73: Troubleshooting And Test Functions

    Agilent 1100 Series Fluorescence Detector Reference Manual Troubleshooting and Test Functions O er ie of the Dete tor’s I di ators a d Test Fu tions Status Indicators Error Messages Wavelength Verification and Calibration The Wavelength Calibration Procedure Test Functions...

  • Page 74: Status Indicators

    (see on page 118). Status Indicators Two status indicators are located on the front of the detector. The lower left indicates the power supply status, the upper right indicates the detector status. 1100 Series FD Reference Manual...

  • Page 75: Power Supply Indicator

    • An error condition is indicated when the status indicator is red. An error condition indicates the detector has detected an internal problem which affects correct operation of the detector. Usually, an error condition requires attention (e.g. leak, defective internal components). An error condition always interrupts the analysis. 1100 Series FD Reference Manual 75...

  • Page 76: Error Messages

    This section describes the meaning of detector error messages, and provides information on probable causes and suggested actions how to correct error conditions. 1100 Series FD Reference Manual...

  • Page 77: Time-Out

    • A not-ready state was present during a sequence or multiple-injection run for a period longer than the time-out threshold. ✔ Suggested Actions Check the logbook for the occurrence and source of a not-ready condition. Restart the analysis where required. 1100 Series FD Reference Manual 77...

  • Page 78: Shutdown

    Check external instruments for a shut-down condition. ✔ Check the degasser for an error condition. Refer to the Reference Manual for the Agilent 1100 Series vacuum degasser. Remote Time-out A not-ready condition is still present on the remote input. When an analysis is started, the system expects all not-ready conditions (e.g. a not- ready condition during detector balance) to switch to run conditions within one minute of starting the analysis.

  • Page 79: Synchronization Lost

    When a leak occurs, the leak sensor is cooled by the solvent. This changes the resistance of the leak sensor which is sensed by the leak-sensor circuit on the FLM board. Probable Causes • Loose fittings. • Broken capillary. • Leaking flow cell. Suggested Actions 1100 Series FD Reference Manual 79...
  • Page 80 4 of the sampler switching valve. This tube can then be taken to waste separately. The tube which normally serves as the detector cell outlet tube can be used for this purpose. 1100 Series FD Reference Manual...

  • Page 81: Leak Sensor Open

    If the current falls outside the lower limit, the error message is generated. Probable Causes • Leak sensor not connected to the FLM board. • Defective leak sensor. Suggested Actions ✔ Ensure the leak sensor is connected correctly. ✔ Exchange the leak sensor. 1100 Series FD Reference Manual 81...

  • Page 82: Leak Sensor Short

    If the current increases above the upper limit, the error message is generated. Probable Causes • Defective leak sensor. Suggested Actions ✔ Exchange the leak sensor. 1100 Series FD Reference Manual...

  • Page 83: Compensation Sensor Open

    If the resistance across the sensor increases above the upper limit, the error message is generated. Probable Causes • Defective FLM board. Suggested Actions ✔ Exchange the FLM board. 1100 Series FD Reference Manual 83...

  • Page 84: Compensation Sensor

    If the resistance across the sensor falls below the lower limit, the error message is generated. Probable Causes • Defective FLF board. Suggested Actions ✔ Exchange the FLF board. 1100 Series FD Reference Manual...

  • Page 85: Fan Failed

    Probable Causes • Fan cable disconnected. • Defective fan. • Defective FLM board. Suggested Actions ✔ Ensure the fan is connected correctly. ✔ Exchange fan. ✔ Exchange the FLM board. 1100 Series FD Reference Manual 85...

  • Page 86: Motor Errors

    FLF board (Ex) or monochromator motor FLM board (Em) power driver defective Table 17 Motor Errors, continued Message Description Probable Causes Suggested Actions 1100 Series FD Reference Manual...
  • Page 87 Wrong interface and recalibrate is checked against a known has a different pattern or EX 6717 pattern no reset of pattern was EM 6718 made encoder lost position replace monochromator completely assembly 1100 Series FD Reference Manual 87...

  • Page 88: Lamp Cover Open

    The lamp cover in the optical compartment has been removed. The lamp cannot be turned on while this message is on. Probable Causes • lamp cover removed. Suggested Actions ✔ close lamp cover and tighten the screws. 1100 Series FD Reference Manual...

  • Page 89: Flf Board Not Found

    • FLF board not connected to the FLM board. • defective FLF board. • defective FLM board. Suggested Actions ✔ Check the connection between the FLF board and the FLM board. ✔ Exchange the FLF board. ✔ Exchange the FLM board. 1100 Series FD Reference Manual 89...

  • Page 90: Adc Not Calibrated

    Troubleshooting and Test Functions ADC Not Calibrated The analog-to-digital converter located on the FLF board cannot calibrate. Probable Causes • defective ADC or other FLF electronics. Suggested Actions ✔ Exchange the FLF board. 1100 Series FD Reference Manual...

  • Page 91: A/D Overflow

    Probable Causes • shortage of flash lamp assembly • shortage of trigger pack assembly. • defective FLL board. Suggested Actions ✔ Exchange the flash lamp assembly. 1100 Series FD Reference Manual 91...
  • Page 92 Troubleshooting and Test Functions ✔ Exchange the FLL board (includes the trigger pack). 1100 Series FD Reference Manual...

  • Page 93: Flash Trigger Lost

    ✔ Reboot the detector (power cycle). ✔ Multi Mode Off: exchange the firmware or replace the main board. ✔ Multi Mode Ex: replace EX monochromator assembly. ✔ Multi Mode Em: replace EM monochromator assembly. 1100 Series FD Reference Manual 93...

  • Page 94: Wavelength Calibration Failed

    “Wavelength Calibration Lost” is displayed and the instrument stays in a Not Ready condition. Probable Causes • Reset of monochromator settings after exchange. • Replacement of FLM board. Suggested Actions ✔ Perform a wavelength calibration. 1100 Series FD Reference Manual...

  • Page 95: Flow Cell Removed 103 No

    NOT READY condition exists. If the flow cell is removed during an analysis, a SHUT DOWN is generated. Probable Causes • Flow cell has been removed during analysis. Suggested Actions ✔ Insert flow cell and turn on the lamp. 1100 Series FD Reference Manual 95...

  • Page 96: Peaks

    A complete wavelength calibration is not always required. In most cases a quick wavelength accuracy verification is sufficient enough, see the table below. 1100 Series FD Reference Manual...
  • Page 97 107 shows the steps performed during the wavelength calibration. The excitation grating and the emission grating are calibrated using Rayleigh stray light from the flow cell or cuvette measured with the photomultiplier tube. 1100 Series FD Reference Manual 97...
  • Page 98 Em rotation scan, full circle" (instrument profile) Em rotation scan, full circle" (instrument profile) Em rotation scan, full circle" (instrument profile) Em rotation scan, full circle" (instrument profile) Emission rotation scan, high resolution, part I 44 s 1100 Series FD Reference Manual...

  • Page 99: Check Of Raman Band Of Water

    7 Run the verification. 8 The FLD will change into the multi-excitation mode with emission wavelength at ± 397 nm and scan in the range of the expected maximum of 350 nm 20 nm. 1100 Series FD Reference Manual 99...
  • Page 100 I terpretatio of the Results The Wa ele gth If the limits are not met, check for on page 125 or perform Cali ratio Pro edure on page 114. NOTE ± 350 nm 3 nm Figure 34 Excitation Spectrum 1100 Series FD Reference Manual...
  • Page 101 397 nm 20 nm. 5 Turn the pump on and flush with water for a few minutes to assure a clean flow cell. Flow rate should be 0.5 to 1 ml/min and the baseline stable. 1100 Series FD Reference Manual 101...
  • Page 102 3 nm. 10 Load the method WLEMTEST. The FLD will change into the multi-excitation mode ± and scan in the range of the expected maximum of 350 nm 20 nm. 11 Repeat steps step 6 step 1100 Series FD Reference Manual...
  • Page 103 Spectrum Range EX 377 - 417 nm step 1 nm EM 330 - 370 nm step 1 nm Store Spectra All w/o signal All w/o signal EX Wavelength 350 nm, ON 350 nm, OFF 1100 Series FD Reference Manual 103...
  • Page 104 Troubleshooting and Test Functions EM Wavelength 397 nm, OFF 397 nm, ON Multi WL Settings Multi EX Multi EM 1100 Series FD Reference Manual...

  • Page 105: The Wavelength Calibration Procedure

    3 Take the syringe and fix the needle to the syringe adapter. 4 Suck about 1.0 ml of the calibration sample into the syringe. 5 Keep the syringe in a horizontal position. 6 Remove t#he needle. 1100 Series FD Reference Manual 105...

  • Page 106: Wavelength Calibration

    Module: System - Tests - FLD - Calibrate. Wa ele gth Cali ratio Failed If the wavelength calibration process fails, refer to NOTE page 101. 2 If a deviation is displayed, press Adjust and OK. The history table will be updated. NOTE 1100 Series FD Reference Manual...

  • Page 107: Verification

    Wavelength Calibration - User Interface Verification 1 Refit the capillary to the flow cell. “Check of Raman Band of Water” 2 Follow the procedure on page 108. Test Functions The light path is shown in Figure 1100 Series FD Reference Manual 107...

  • Page 108: Lamp Intensity Test

    1 nm steps) and stores it in a diagnosis buffer. The scan is displayed in a graphic window. There is no further evaluation of the test. Results of this test are stored as lamp history (date code, intensity). 1100 Series FD Reference Manual...

  • Page 109: Lamp Intensity History

    (date code, intensity of four different wavelengths, 250 nm, 350 nm, 450 and 600 nm) in a buffer. The data/plot can be retrieved via the diagnostics and provides intensity data over a length of time. 1100 Series FD Reference Manual 109...

  • Page 110: Dark-Current Test

    It also reads the signal of the reference diode. The resulting values (two via reference diode and two from PMT) are shown in a table and checked against reasonable limits (see below). Figure 45 Dark-Current Test Dark-Current Test Evaluation 1100 Series FD Reference Manual...

  • Page 111: Excitation And Emission Grating Resistance History

    The history data contains the data/time information and the number of turns. The data/plot can be retrieved via the diagnostics. Figure 46 Resistance History Friction Evaluation Motor Error 1100 Series FD Reference Manual 111...

  • Page 112: Raman Astm Signal-To-Noise Test

    Flow rate 0.5 - 1 ml/min ASTM Noise and drift at 350/397 nm, PMT=12 and Responsetime=8 s taken from 5 to 20 minutes Dark current at 350/450 nm and PMT=12 Figure 47 Raman ASTM Signal-to-Noise Test 1100 Series FD Reference Manual...
  • Page 113 Assure that the FLD signal is signal 1 (in case you use an additional detector in the system and your are using a ChemStation older than A.09.xx. Otherwise wrong calculations may be done due to wrong signals. 1100 Series FD Reference Manual 113...

  • Page 114: Using The Built-In Test Chromatogram

    ChemStation and the data analysis or via the analog output to the integrator or data system. An example is shown in Figure 49. The chromatogram is continuously repeated until a stop is executed either by means of a stop time or manually. 1100 Series FD Reference Manual...
  • Page 115 1 Load the FLD default parameter • peakwidth to >0.2 minutes (standard), • set stop time to 4.8 minutes. 2 Complete the Sample Information (no injection). 3 Type into the command line (or as pre-run command): PRINT SENDMODULE$(LFLD,"SIMU:DFLT"). 1100 Series FD Reference Manual 115...

  • Page 116: Using The Built-In Dac Test

    The test chromatogram is switched off automatically at the end of the run. NOTE Using the Built-in DAC Test This function is available from the Control Module ONLY. The DAC test provides a test pattern as an analog output. The output voltages 1100 Series FD Reference Manual...
  • Page 117 2 Start the plot mode (e.g. Agilent 3396 with ATTN -4, ZERO=50, CS=5). 3 Stop the plot and disable the TAC Test (System - Tests - FLD - Disable DAC Test Pattern). 4 Evaluate the noise (should be< 5 µV). 1100 Series FD Reference Manual 117...
  • Page 118 Troubleshooting and Test Functions 1100 Series FD Reference Manual...

  • Page 119: Repairing The Fluorescence Detector

    Agilent 1100 Series Fluorescence Detector Reference Manual Repairing the Fluorescence Detector Introduction into Repairing the Fluorescence Detector Overview of the Repairing of the Fluorescence Detector Simple Repairs Exchanging Internal Parts...

  • Page 120: Introduction Into Repairing The Fluorescence Detector

    Electronic boards and components are sensitive to electronic discharge (ESD). In CAUTION order to prevent damage always use an ESD protection (for example, the ESD wrist 1100 Series FD Reference Manual...
  • Page 121 2 Unroll the rest of the band and peel the liner from the copper foil at the opposite end. 3 Attach the copper foil to a convenient and exposed electrical ground. 1100 Series FD Reference Manual 121...
  • Page 122 Repairing the Fluorescence Detector Figure 51 Using the ESD Strap 1100 Series FD Reference Manual...

  • Page 123: Overview Of The Repairing Of The Fluorescence Detector

    Repairing the Fluorescence Detector Overview of the Repairing of the Fluorescence Detector Figure 52 shows the main assemblies and their locations. page 137 Leak sensor, see page 166 Figure 52 Main Assemblies 1100 Series FD Reference Manual 123...

  • Page 124: Simple Repairs

    Cuvette for off-line measurements, 8 µl, 20 bar, G1321-60007, refer to Ho to use the Cu ette on page 140 for more information on usage. DO NOT install the inlet capillary to the outlet connection of the flow cell. This will result in poor performance. 1100 Series FD Reference Manual...
  • Page 125 Repairing the Fluorescence Detector NOTE ü Preparations for this procedure: • Turn off the flow. 1100 Series FD Reference Manual 125...
  • Page 126 LC-MSD. Otherwise the back pressure generated by the other detector may overload the quartz flow cell and will lead to a defective cell (maximum pressure is 20 bar (2 MPa). Always use the outlet capillary set supplied with the accessory kit. 1100 Series FD Reference Manual...

  • Page 127: How To Use The Cuvette

    3 Use the syringe (see on page 214) to inject the compound. 4 Setup the parameters for the Fluorescence Scan (under Special Setpoints). 5 Select “Take Fluorescence Scan” on the user-interface to start the off-line measurement. 1100 Series FD Reference Manual 127...

  • Page 128: Flow Cell Flushing

    Do not exceed the pressure limit of 20 bar (0.2 MPa). NOTE Correcting Leaks When required If a leakage has occurred in the flow cell area or at the capillary connections Tools required Tissue Two 1/4 inch wrenches for capillary connections Parts required None 1100 Series FD Reference Manual...

  • Page 129: Replacing Leak Handling System Parts

    Tools required None Parts required Leak funnel 5061-3356 Leak funnel holder 5041-8389 Leak tubing (120 mm) 0890- 1711 1 Remove the front cover. 2 Pull the leak funnel out of the leak funnel holder. 1100 Series FD Reference Manual 129...

  • Page 130: Exchanging Internal Parts

    WARNING To disconnect the detector from line, unplug the power cord. The power supply still uses some power, even if the switch on the front panel is turned off. 1100 Series FD Reference Manual...
  • Page 131 133. Eye damage may result from directly viewing the light produced by the xenon flash WARNING lamp used in this product. 1100 Series FD Reference Manual 131...

  • Page 132: Removing The Covers

    When required For all repairs inside the detector Tools required Screwdriver POZI 1 PT3 Parts required Depends on the work inside and the following procedures CAUTION There will be a risk of damaging hardware due to overheating when operating the instrument without covers. 1100 Series FD Reference Manual...

  • Page 133: Removing The Rear Foam

    Depends on the work inside and the following procedures Preparations for this procedure: Using a pliers disconnect the cables from the main board. • Re o i g the Co ers Start with page 146. 1100 Series FD Reference Manual 133...
  • Page 134 Install the ESD strap. Move the power lock across the power inlet and lift the clips on the rear of the cover. Repairing the Fluorescence Detector 1100 Series FD Reference Manual...

  • Page 135: Exchanging The Lamp

    The instrument should not be operated without Xenon flash lamp. Otherwise the Triggerpack electronics will be damaged. NOTE When loosening or removing screws take care that they do not fall into the instrument. This may result in a complete removal of other assemblies. 1100 Series FD Reference Manual 135...
  • Page 136 Remove the flow cell or disconnect the tubings from the flow cell. • Remove detector from stack and place it on the workbench. • Remove the covers as described in Re o i g the Co ers on page 146. 1100 Series FD Reference Manual...
  • Page 137 Repairing the Fluorescence Detector 1100 Series FD Reference Manual 137...
  • Page 138 WARNING: While pulling off the lamp be careful that you do not scrape your skin on the metal plates. Do not remove the bottom pad. Otherwise the lamp will loose its correct position during reinstallation. 1100 Series FD Reference Manual...
  • Page 139 Note: Using the 2.5 mm hexagonal key, unscrew the two screws and remove the brass pad together with its holder. unscrew Repairing the Fluorescence Detector grounding screw (marked with X) 1100 Series FD Reference Manual 139...
  • Page 140 Repairing the Fluorescence Detector 7 Remove the lamp carefully from the trigger 8 Carfully insert the new lamp completely into the pack. trigger pack and slide the cables through the holder. 1100 Series FD Reference Manual...
  • Page 141 Repairing the Fluorescence Detector 1100 Series FD Reference Manual 141...

  • Page 142: Exchanging The Ex-Condenser

    Repairing the Fluorescence Detector Exchanging the EX-condenser When required Condenser: if contaminated WARNING 1100 Series FD Reference Manual...
  • Page 143 Remove the flow cell or disconnect the tubings from the flow cell. • Remove detector from stack and place it on the workbench. • Remove the covers as described in Re o i g the Co ers on page 146. 1100 Series FD Reference Manual 143...
  • Page 144 Repairing the Fluorescence Detector 1100 Series FD Reference Manual...
  • Page 145 Repairing the Fluorescence Detector Using a 2.5 mm hexagonal key, remove the loosen condenser. condenser. the screw There is mechanical stop for 1100 Series FD Reference Manual 145...
  • Page 146 Turn the lamp on. • Perform a wavelength verification to check the correct Rear positioning of the replaced foam assemblies, as described in chapter Wa ele gth Verifi atio a d Cali ratio on page 105. 1100 Series FD Reference Manual...

  • Page 147: Replacing The Lamp Cover Window

    Remove the flow cell or disconnect the tubings from the flow cell. Disconnect the emission and the • Remove detector from stack and place excitation cables and from the it on the workbench. detector main board. 1100 Series FD Reference Manual 147...
  • Page 148 Repairing the Fluorescence Detector • Remove the covers as described in Re o i g the Co ers on page 146. 1100 Series FD Reference Manual...
  • Page 149 Repairing the Fluorescence Detector Note: The quartz window may be cleaned with alcohol (e.g. ethanol). 1100 Series FD Reference Manual 149...
  • Page 150 Repla i g the Foa a d the Top the main board. Left is excitation, right is emission. Co er o page 4 . • Re-install the detector in the stack. • Turn the lamp on. Rear foam 1100 Series FD Reference Manual...

  • Page 151: Exchanging The Processor Board

    Detector main board (FLM) G1321-69500 ( exchange assembly ) 1 Turn off the lamp. 2 Switch off the module, and disconnect the cables. 3 Remove module from stack and place it on the workbench. Figure 55 Unscrew Connectors from Board 1100 Series FD Reference Manual 151...
  • Page 152 (yellow or red flashing status light). In this case turn off the module, reset the address switches, and turn on the module again. 9 Install the new processor board and reconnect the connectors. Assure that the board is fitted correctly into the board recess in the rear panel. 1100 Series FD Reference Manual...
  • Page 153 Module serial numbers are entered by typing specific commands in the command line at the bottom of the main user interface screen. 1 To enter a module serial number, type the following command in the command line: print sendmodule$(lfld,"ser YYYYYYYYYY") 1100 Series FD Reference Manual 153...

  • Page 154: Exchanging The Fan

    When required If the fan is defective or noisy Tools required Screwdriver POZI 1 PT3 Parts required Fan assembly 3160-1017 CAUTION The fan must be installed in the correct orientation to ensure optimum cooling and operation of the detector. 1100 Series FD Reference Manual...
  • Page 155 Remove the covers as described in Re o i g the Co ers on page 146. Carefully remove the rear foam. Lift the main board slightly. Bring the fan cable up and disconnect the fa Pull out the fan. 1100 Series FD Reference Manual 155...
  • Page 156 Next Steps: • Repla e the o ers as des ri ed i Repla i g the Foa a d the Top Co er o page 4 . • Re-install the detector in the stack. 1100 Series FD Reference Manual...

  • Page 157: Exchanging The Leak Sensor Or Leak Panel

    Rear foam Exchanging the Leak Sensor or Leak Panel When required If defective Tools required Screwdriver POZI 1 PT3 Flat screwdriver Leak sensor assembly 5061- Parts required 3356 Leak Pan G1321-45501 1100 Series FD Reference Manual 157...
  • Page 158 Re o i g the Co ers Remove the covers as described in on page 146. • Remove the flow cell. Disconnect the Pull out the leak sensor leak sensor. cable using your left hand. 1100 Series FD Reference Manual...
  • Page 159 Repairing the Fluorescence Detector Note: Using flat screw driver, release the leak base (two clasps). If you want to replace just the leak sensor, continue with step 1100 Series FD Reference Manual 159...

  • Page 160: Replacing The Em-Condenser Or Cutoff-Filter

    Replace the covers as described in on page • • 196. Re-install the flow cell and the front panel Re-install the detector in the stack. Replacing the EM-Condenser or Cutoff-Filter When required If light throughput is too low 1100 Series FD Reference Manual...
  • Page 161 Remove the flow cell. • Remove detector from stack and place it on the workbench. • Remove the covers as described in Re o i g the Co ers on page 146. • Remove the flow cell. 1100 Series FD Reference Manual 161...
  • Page 162 Repairing the Fluorescence Detector 1100 Series FD Reference Manual...
  • Page 163 Turn the lamp on. • Perform a wavelength verification to check the correct positioning of the replaced assemblies, as described in Wa ele gth Verifi atio a d Cali ratio chapter on page 105. 1100 Series FD Reference Manual 163...

  • Page 164: Replacing The Mirror Assembly

    Mirror assembly 1000-1000 DO NOT touch the surface of any optical component during this procedure. This will reduce the reflection efficiency. O e side of the irror is arked R represe ti g the rear side. NOTE 1100 Series FD Reference Manual...
  • Page 165 Disconnect the power cable. • Remove the flow cell. • Remove detector from stack and place it on the workbench. • Remove the covers as described in Re o i g the Co ers on page 146. 1100 Series FD Reference Manual 165...
  • Page 166 Repairing the Fluorescence Detector Locate the mirror assembly. Use a pair 1100 Series FD Reference Manual...
  • Page 167 Repairing the Fluorescence Detector Note: 1100 Series FD Reference Manual 167...
  • Page 168 The Repairing the Fluorescence Detector towards mirror the light. surface The back this side! If the mirror is inserted in the opposite direction, the detector cannot be aligned correctly. 1100 Series FD Reference Manual...
  • Page 169 Repairing the Fluorescence Detector 1100 Series FD Reference Manual 169...

  • Page 170: Replacing The Slits

    Disconnect the power cable. • Remove the flow cell. • Remove detector from stack and place it on the workbench. • Re o i g the Remove the covers as described in Co ers on page 146. 1100 Series FD Reference Manual...
  • Page 171 Replace the UV protector and the front foam. • • Repla i g the Foa s a d Co ers Replace the covers as described in on page 196. Re-install the flow cell and the front panel 1100 Series FD Reference Manual 171...

  • Page 172: Removing The Optical Unit

    Disconnect the power cable. • Disconnect capillaries. • Remove detector from stack and place Disconnect cables it on the workbench. monochromator) tector main board monochromator) from the de (FLM). procedure. Otherwise parts can fall out. 1100 Series FD Reference Manual...
  • Page 173 Repairing the Fluorescence Detector • Remove the covers as described in Re o i g the Co ers on page 146. • Remove the flow cell. 1100 Series FD Reference Manual 173...
  • Page 174 Repairing the Fluorescence Detector 1100 Series FD Reference Manual...
  • Page 175 3 Disconnect the leak sensor cable (J3) and unsc Rear foam Screw 4 Disconnect the optical unit 5 Remove the optical unit and place it on the ben cable (J20). required). cable (J18) and the EM motor 1100 Series FD Reference Manual 175...

  • Page 176: Replacing Pmt And/Or Flf Board

    Hamamatsu dealers. Alternative PMTs are either R928HA (185 to 900 nm) or R3788HA (185 to 750 nm). No other PMTs are recommended. FLF Board G1321-69531 (requires firmware revision A.04.06 or above), FLR Reference Diode board G1321-66533 CAUTION 1100 Series FD Reference Manual...
  • Page 177 Repairing the Fluorescence Detector When working on the optical unit, a clean workbench with ESD protection mat must be available. Otherwise optical components or electronic boards may be damaged. 1100 Series FD Reference Manual 177...
  • Page 178 Repairing the Fluorescence Detector 2 Unscrew screws A and B and disconnect connectors C and D. Disc a fla 1100 Series FD Reference Manual...
  • Page 179 Repairing the Fluorescence Detector 1100 Series FD Reference Manual 179...
  • Page 180 8 Replace the FLF board and fix the screws (A and B) and connectors (C and D). 9 Check that the sa board and castin Repairing the Fluorescence Detector Next Steps: 1100 Series FD Reference Manual...

  • Page 181: Replacing Fll Board And Trigger Pack

    When working on the optical unit, a clean workbench with ESD protection mat must be available. Otherwise optical components or electronic boards may be damaged. CAUTION The instrument should not be operated without Xenon flash lamp. Otherwise the WARNING Triggerpack electronics will be damaged. 1100 Series FD Reference Manual 181...
  • Page 182 Optical unit has been removed as described in Re o i g the Opti al U it on page 178. • The foam must be in place. Otherwise cutoff filter and diffuser will fall out. 1100 Series FD Reference Manual...
  • Page 183 Repairing the Fluorescence Detector Carefully pull wires off the ferret from safe keep it place. Then in a and the pull out the Ferret. FLL board. FLL Board FLL Board Ferret 1100 Series FD Reference Manual 183...
  • Page 184 Repairing the Fluorescence Detector 8 Put the wires into the released contacts using the tweezers. Order of wires (left to right): 1100 Series FD Reference Manual...
  • Page 185 • Turn the lamp • Perform a Rear wavelength foam verification to check the correct positioning of the replaced assemblies, as described in chapter Wa ele gth Verification and Cali ratio page 105. 1100 Series FD Reference Manual 185...
  • Page 186 Repairing the Fluorescence Detector 1100 Series FD Reference Manual...

  • Page 187: Replacing The Em And Ex Grating

    (at the rear of the EM or EX grating assembly) should be disconnected. • Disconnect the encoder cable of the EX-monochromator from FLF board. protection ring. DO NOT touch the grating surface and DO NOT bend the protection ring. 1100 Series FD Reference Manual 187...
  • Page 188 Repairing the Fluorescence Detector 1100 Series FD Reference Manual...
  • Page 189 Repairing the Fluorescence Detector 1100 Series FD Reference Manual 189...
  • Page 190 Repairing the Fluorescence Detector Next Steps: • Reconnect the encoder cable of the EX-monochromator to FLF board. 1100 Series FD Reference Manual...

  • Page 191: Exchanging The Power Supply

    Screwdriver POZI 1 PT3 Wrench 1/4 inch NOTE Wrench 5 mm Wrench 7 mm Parts required Power supply 0950- 2528 The repair of the power supply assembly comprises exchanging the complete assembly. No serviceable parts are inside. 1100 Series FD Reference Manual 191...
  • Page 192 Re o i g the Opti al U it Remove the optical unit, see on page 178. 2 Unscrew the power supply at the rear of the module. 1 Carefully remove the bottom foam piece by sliding it out towards the rear. 1100 Series FD Reference Manual...
  • Page 193 Repairing the Fluorescence Detector The repair of the power supply assembly is comprised of exchanging the complete assembly. No serviceable parts are inside. 1100 Series FD Reference Manual 193...

  • Page 194: Replacing Status Light Pipe

    12 Replace detector into the stack. 13 Reconnect the power cable and turn on the detector. Replacing Status Light Pipe When required If part was broken or removed Tools required Screwdriver POZI 1 PT3 Parts required Status light pipe 5041-8384 1100 Series FD Reference Manual...

  • Page 195: Installing The Optical Unit

    1 Place the optical unit in the instru Preparations for this procedure: grounding screw. • All previous work has been completed. • Power supply has been installed. • Fan has been installed. • The optical unit has its foam cover attached. 1100 Series FD Reference Manual 195...
  • Page 196 Repairing the Fluorescence Detector Screw 2 Reconnect the leak sensor cable (J3) using your left hand. 3 Reconnect the optical unit cable ( (J20). 1100 Series FD Reference Manual...
  • Page 197 4 Insert the rear foam and reconnect cables (EM monochromator) panel and (EX monochromator) to the detector main board (FLM). • Re-install the detector in the stack. • Turn the lamp on. • Perform a wavelength verification to check the correct 1100 Series FD Reference Manual 197...

  • Page 198: Replacing The Foams And Covers

    Ne t Steps o page 189. When required When all repairs have been completed Tools required Screwdriver POZI 1 PT3 Prerequisites The detector is open and other procedures have been carried out NOTE 1100 Series FD Reference Manual...
  • Page 199 Repairing the Fluorescence Detector The front cover (across the optical unit) should only be removed when required during a procedure. This will keep dust away from optical components. Carefully insert the rear foam. Rear 1100 Series FD Reference Manual 199...
  • Page 200 Repairing the Fluorescence Detector 1100 Series FD Reference Manual...

  • Page 201: Assembling The Main Cover

    Replace the detector into the stack and Reinstall the flow cell. • Reconnect the power cable and turn on the detector. • Turn the lamp on. Assembling the Main Cover When required If cover is broken 1100 Series FD Reference Manual 201...
  • Page 202 1 sides into the top part. Place the top part on the bench and insert the left and right Next steps: • Replace the detector in the stack and reconnect the cables and capillaries. • Turn on the detector. 1100 Series FD Reference Manual...

  • Page 203: Replacing The Interface Board

    • if new version solves problems of currently installed version, or • if after exchange of the main board (FLM) the version on board is older than the previously installed one. To upgrade the detector’s firmware the following steps have to be taken: 1100 Series FD Reference Manual 203...
  • Page 204 2 If FLM board was replaced, reenter the serial number information of the module “Entering the Serial Number using the Control through the user interface, see Module” “Entering the Serial Number using the Agilent on page 162 or ChemStation” on page 163. 1100 Series FD Reference Manual...

  • Page 205: Identifying Parts And Materials

    Agilent 1100 Series Fluorescence Detector Reference Manual Identifying Parts and Materials Overview of Main Assemblies Optical Unit Assembly Lamp Cover Parts Control Module Sheet Metal Kit Plastic Parts Foam Parts Power and Status Light Pipes Leak Parts Cuvette Kit Spare Parts...

  • Page 206: Overview Of Main Assemblies

    Identifying Parts and Materials Agilent Technologies Overview of Main Assemblies Figure 58 shows the main assemblies and their locations. Figure 58 Main Assemblies Table 24 Main Assemblies Item Description Part Number 1100 Series FD Reference Manual...
  • Page 207 Hexagonal nut for RS-232C connector 1251-7788 Nut for analog connector 2940-0256 Washer for analog connector 2190-0699 Cable CAN to Agilent 1100 Series modules (0.5 m), see page 233 5181-1516 Power supply for power and status light parts, see page 212 0950-2528...

  • Page 208: Optical Unit Assembly

    Slit (EM) 2x8 G1321-08102 Photomuliplier tube assembly (PMT), see also page 180 for additional information 1970-0201 Condenser Emission 1000-1124 Front-end Board (FLF), underneath the optical (exchange assembly) (requires firmware G1321-69531 revision A.04.06 or above ) 1100 Series FD Reference Manual...
  • Page 209 Screw M5 x 25 mm, for chassis cable 0515-2574 Screw 2.5 mm hex, for monochromator, lamp pad, condenser #1, slits, etc. 0515-1052 Screw M4 x 25 mm hex, for lamp housing 0515-2548 Screw M4 x 8 mm, for FLF board 0515-2549 1100 Series FD Reference Manual 209...

  • Page 210: Lamp Cover Parts

    Identifying Parts and Materials Figure 59 Optical Unit Parts Lamp Cover Parts Table 26 Lamp Cover Parts Item Description Part Number Plate G1321-08100 1100 Series FD Reference Manual...

  • Page 211: Control Module

    Table 27 Control Module Parts Item Description Part Number Control Module, replacement part including cable G1323-67001 Plastic Housing Kit, includes front, back and a clamp 5062-8583 CAN cable Agilent 1100 module to control module G1323-81600 1100 Series FD Reference Manual 211...

  • Page 212: Sheet Metal Kit

    Figure 61 Control Module Sheet Metal Kit Table 28 Sheet Metal Kit Parts Item Description Part Number Sheet metal kit includes case and top cover G1321-68701 Screws M3 for cover and flow cell door 5022-2112 1100 Series FD Reference Manual...

  • Page 213: Plastic Parts

    Identifying Parts and Materials Plastic Parts Table 29 Plastics Parts NOTE Item Description Part Number Front cover 5062-8582 Plastics, includes base, sides and top 5062-8565 Name plate Agilent 1100 Series 5042-1381 1100 Series FD Reference Manual 213...

  • Page 214: Foam Parts

    EPP foam kit, includes bottom and top rear G1321-68702 Foam Pads (located underneath the optical), set of two G1321-68700 Guides for interface board 5041-8395 Do not order the individual part numbers imprinted on the NOTE foam. 1100 Series FD Reference Manual...

  • Page 215: Power And Status Light Pipes

    Part Number Power supply assembly 0950-2528 Screw M4 x 0.7, 8 mm lg, to fix power supply at rear panel 0515-0910 Washer 2190-0409 Power light pipe 5041-8382 Status light pipe 5041-8384 Power switch button 5041-8381 1100 Series FD Reference Manual 215...

  • Page 216: Leak Parts

    Description Part Number Leak sensor assembly 5061-3356 Leak pan G1321-45501 Leak funnel 5041-8388 Leak funnel holder 5041-8389 Corrugated tubing, 120 mm lg, re-order 5 m 5062-2463 Corrugated tubing, 1200 mm lg, re-order 5 m 5062-2463 1100 Series FD Reference Manual...

  • Page 217: Cuvette Kit

    Part Number FLD Cuvette Kit, 8 µl, 20 bar G1321-60007 includes Tubing, flexible, 1 meter SST Fitting, QTY=1 79814-22406 SST front ferrule, QTY=1 0100-0043 SST back ferrule, QTY=1 0100-0044 PEEK fitting, QTY=1 0100-1516 Needle-Syringe 9301-0407 1100 Series FD Reference Manual 217...

  • Page 218: Spare Parts

    Photo-multiplier Tube (PMT) R3788HA (185 to 750 nm) Accessory Kit This kit contains some accessories and tools needed for the installation and repair/calibration of the detector. Table 35 Accessory Kit Parts Item Description Part Number 1100 Series FD Reference Manual...
  • Page 219 5063-6597 Sample filter, diameter=3 mm, pore size 0.45 µm, QYT=5 5061-3367 (pack of 100) Hex key set 1 – 5 mm 8710-0641 Wrench open end 1/4 – 5/16 inch 8710-0510 ESD wrist strap 9300-1408 1100 Series FD Reference Manual 219...

  • Page 220: Cable Overview

    This end is pre-installed Figure 68 Inlet Capillary (Column-Detector) Parts Cable Overview WARNING Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations. Table 36 Cables Overview Type...
  • Page 221 HP 1090 liquid chromatographs 01046-60202 Signal distribution module 01046-60202 Table 36 Cables Overview, continued Type Description Part Number 3396 integrator 03396- cables 60560 General purpose (spade Lugs) G1351- 81600 Auxiliary Agilent 1100 Series vacuum degasser G1322- 61600 1100 Series FD Reference Manual 221...

  • Page 222: Analog Cables

    5181-1516 cables Agilent 1100 module to module, 1 m 5181-1519 Agilent 1100 module to control G1323- module 81600 External Agilent 1100 Series interface board G1103- contacts to general purpose 61611 GPIB Agilent 1100 module to Agilent 10833 A cable ChemStation, 1 m...
  • Page 223 Analog - Connected to pin 4 Not connected Agilent 1100 to 3394/6 Integrators Connector Signal Name 35900-60750 3394/6 Agilent 1100 Not connected Shield Analog - Center Analog + Agilent 1100 to BNC ctor Conne 1100 Series FD Reference Manual 223...
  • Page 224 Identifying Parts and Materials Connector Signal Name 8120-1840 Agilent 1100 Shield Shield Analog - Center Center Analog + Agilent 1100 to General Purpose Connector Signal Name 01046-60105 3394/6 Agilent 1100 Not connected Black Analog - Analog + 1100 Series FD Reference Manual...

  • Page 225: Remote Cables

    Remote Cables One end of these cables provides a Agilent Technologies APG (Analytical Products Group) remote connector to be connected to Agilent 1100 Series modules. The other end depends on the instrument it is to be connected to. Agilent 1100 to 3390 Integrators...
  • Page 226 3 - Gray Start 4 - Blue Shut down 5 - Pink Not connected 6 - Yellow Power on High 4 - Key 7 - Red Ready High 8 - Green Stop 9 - Black Start request 1100 Series FD Reference Manual...
  • Page 227 START and STOP are connected via diodes to pin 3 of the 3394 connector. NOTE Agilent 1100 to 3396A Integrators Connector Signal Name Active 03394-60600 3394 Agilent 1100 ( TTL ) 1 - White Digital ground 2 - Brown Prepare run 3 - Gray Start 1100 Series FD Reference Manual 227...
  • Page 228 Prepare run 3 - Gray Start 4 - Blue Shut down 5 - Pink connected 6 - Yellow Power on High 7 - Red Ready High 8 - Green Stop 9 - Black Start request 1100 Series FD Reference Manual...
  • Page 229 Signal Distr ibution Modul e LC or Connector Signal Name Active 01046-60202 HP 1090 Agilent 1100 ( TTL ) 1 - White Digital ground 2 - Brown Prepare run 3 - Gray Start 4 - Blue Shut down 1100 Series FD Reference Manual 229...
  • Page 230 Prepare run 3 - Gray Start 4 - Blue Shut down 5 - Pink connected 6 - Yellow Power on High 7 - Red Ready High 8 - Green Stop 9 - Black Start request 1100 Series FD Reference Manual...

  • Page 231: Bcd Cables

    Identifying Parts and Materials BCD Cables One end of these cables provides a 15-pin BCD connector to be connected to the Agilent 1100 Series modules. The other end depends on the instrument it is to be connected to Agilent 1100 to General Purpose...

  • Page 232: Auxiliary Cable

    Auxiliary Cable One end of this cable provides a modular plug to be connected to the Agilent 1100 Series vacuum degasser. The other end is for general purpose. Agilent 1100 Series Degasser to general purpose 1100 Series FD Reference Manual...

  • Page 233: Can Cable

    DC + 5 V IN Pink Vent CAN Cable Both ends of this cable provide a modular plug to be connected to Agilent 1100 Series module’s CAN-bus connectors. Agilent 1100 module to module, 0.5 m 5181-1516 Agilent 1100 module to module, 1 m...

  • Page 234: External Contact Cable

    Identifying Parts and Materials External Contact Cable One end of this cable provides a 15-pin plug to be connected to Agilent 1100 Series module’s interface board. The other end is for general purpose. Agilent 1100 Series Interface Board to general purpose...

  • Page 235: Rs-232 Cable Kit

    RS-232 Cable Kit This kit contains a 9-pin female to 9-pin female Null Modem (printer) cable and one adapter. Use the cable and adapter to connect Agilent Technologies instruments with 9- pin male RS-232 connectors to most PCs or printers.
  • Page 236 Identifying Parts and Materials Cross-over network cable (shielded, 3 m long), 5023- 0203 ( for point to point connection ) Twisted pair network cable (shielded, 7 m long) ( 5023- for hub connections ) 0202 1100 Series FD Reference Manual...

  • Page 237: Introduction To The Fluorescence Detector

    Agilent 1100 Series Fluorescence Detector Reference Manual Introduction to the Fluorescence Detector Introduction to the Detector How the Detector Operates Raman Effect Optical Unit Analytical Information From Primary Data Electrical Connections Instrument Layout Early Maintenance Feedback (EMF)

  • Page 238: Introduction To The Detector

    • optional cuvette is available and can be used for off-line measurements • easy front access to flow cell for fast replacement and • built-in wavelength accuracy verification. “Performance Specifications” For specifications, see on page 330 Figure 69 The Agilent 1100 Series Fluorescence Detector. 1100 Series FD Reference Manual...

  • Page 239: How The Detector Operates

    Figure 71. The characteristic maxima of absorption for a substance is its λ , and for emission its λ 1100 Series FD Reference Manual 239...
  • Page 240 Phosphorescence is a longer process because one of the electrons involved in the excitation changes its spin, during a collision with a molecule of solvent, for example. The excited molecule is now in a so-called triplet state, T, see Figure 1100 Series FD Reference Manual...

  • Page 241: Raman Effect

    While most of this scattered light is at the same wavelength as the incident light, some is scattered at a different wavelength. This inelastically scattered light is called Raman scatter. It results from the molecule changing it's molecular motions. 1100 Series FD Reference Manual 241...

  • Page 242: Optical Unit

    The fluorescence detector has grating/grating optics, enabling the selection of both excitation and emission wavelengths. The flow cell can be accessed from the front of the fluorescence detector. 1100 Series FD Reference Manual...
  • Page 243 UV degradation, especially below 250 nm is significantly higher compared to Visible wavelength range. Generally the "LAMP ON during run" - setting or using "economy mode" will increase lamp life by a magnitude. 1100 Series FD Reference Manual 243...
  • Page 244 Figure 76 Mirror Assembly The geometry of the grooves is optimized to reflect almost all of the incident light, in the 1 order and disperse it with about 70% efficiency in the ultra-violet range. Most 1100 Series FD Reference Manual...
  • Page 245 The flow cell is a solid quartz body with a maximum back pressure of 20 bar. Excessive back pressure will result in destruction of the cell. Operating the detector close to waste with low back pressure is recommended. A slit is integrated to the quartz body. 1100 Series FD Reference Manual 245...
  • Page 246 The amplification is a function of the voltage at the dynodes and is microprocessor controlled. You can set the amplification using the PMTGAIN function. 1100 Series FD Reference Manual...

  • Page 247: Reference System

    A diffuser is located in front of the reference diode (see Figure 74 on page 244). This diffuser is made of quartz, reduces light and allows integral measurement of the light. 1100 Series FD Reference Manual 247...

  • Page 248: Analytical Information From Primary Data

    Figure 80 Measurement of Fluorescence Phosphorescence Detection An appropriate parameter set will be specified as soon as you chose the phosphorescence detection mode (special setpoints under FLD parameter settings). 1100 Series FD Reference Manual...

  • Page 249: Of Raw Data

    296 times per second. If the “economy” or multi-wavelength mode is set, then the flash frequency is 74 Hz. Figure 82 LAMP: Frequency of Flash, Fluorescence, and Phosphorescence 1100 Series FD Reference Manual 249...
  • Page 250 After the photons are converted and multiplied into an electronic signal, the signal (at present analog) is tracked and held beyond the photo-multiplier. After being held, the signal is converted by an A-to-D converter to give one raw data point (digital). Eleven 1100 Series FD Reference Manual...

  • Page 251: Electrical Connections

    GPIB connector determines the GPIB address “GPIB Default of your detector. The switches are preset to a default address (see Addresses” on page 293) which is recognized once the power is switched on. 1100 Series FD Reference Manual 251...
  • Page 252 Introduction to the Fluorescence Detector • The CAN bus is a serial bus with high speed data transfer. The two connectors for the CAN bus are used for internal Agilent 1100 Series module data transfer and synchronization. • Two independent analog outputs provide signals for integrators or data handling systems.

  • Page 253: Instrument Layout

    • the plastic layers help cushion the electronic and mechanical parts from physical shock, and • the metal inner cabinet shields the internal electronics from electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself. 1100 Series FD Reference Manual 253...

  • Page 254: Early Maintenance Feedback (Emf)

    296 Hz (Standard), 560 V 63 mJoule (18.8 W) 74 Hz (Economy), 560 V 63 mJoule (4.7 W) Rotation (Multi Ex/Em) 74 Hz (Standard), 950 V 180 mJoule (13.3 W) 74 Hz (Economy), 560 V 63 mJoule (4.7 W) 1100 Series FD Reference Manual...

  • Page 255: Using The Emf Counters

    (or values slightly less than the displayed values) as EMF limits, and then reset the EMF counters to zero. The next time the EMF counters exceed the new EMF limits, the EMF flag will be displayed, providing a reminder that maintenance needs to be scheduled. 1100 Series FD Reference Manual 255...
  • Page 256 Introduction to the Fluorescence Detector 1100 Series FD Reference Manual...

  • Page 257: Theory Of Operation

    Agilent 1100 Series Fluorescence Detector Reference Manual 8 Theory of Operation Electronics Detector Main Board (FLM) Detector Frontend Board (FLF) Detector Lamp Supply Board (FLL) Firmware Description Raw Data Conversion to Fluorescence (LU) Units Optional Interface Boards Interfaces Setting the 8-bit Configuration Switch...

  • Page 258: Electronics

    • detector frontend board (FLF), see page 269. • detector lamp board (FLL), see page 275. • power supply, see page 297. Optional: • interface board (BCD/external contacts), see page 284. • interface board (LAN), see page 286. 1100 Series FD Reference Manual...

  • Page 259: Detector Main Board (Flm)

    The 304-pin application specific integrated circuit (ASIC) provides interfacing to external devices through drivers, including LAN, GPIB, CAN, APG remote, and RS- 232C. It is connected directly to the four control LEDs located near the connectors on 1100 Series FD Reference Manual 259...
  • Page 260 A chopped motor driver IC provides the signal to run the excitation/emission monochromator motor in positioning or rotation mode. Encoder Signal Acquisition Each monochromator includes an optical encoder to get the actual position of the device. The two encoder signals are amplified and prepared for A/D-conversion. 1100 Series FD Reference Manual...
  • Page 261 The operation of the fan is controlled by the main processor and runs with constant revolution. The fan produces a sense signal which is derived from the revolution. This sense signal is used for diagnostics. 1100 Series FD Reference Manual 261...

  • Page 262: Detector Frontend Board (Flf)

    • monochromator positions • board temperature • leak sensor status Then the digital data are polled by the FPGA on the FLM main board to be available for calculations. 1100 Series FD Reference Manual...
  • Page 263 Flash Voltage Safety Switch A safety switch stops the voltage regulator when the lamp cover is removed to avoid high voltages on board when electronic parts are accessible. Photomultiplier Tube Voltage Supply 1100 Series FD Reference Manual 263...
  • Page 264 A reference photodiode is located behind the cell and monitors the incoming radiation through a diffusor window. The data are used to compensate the fluorescence data for drift effects. The reference path provides multiple gain stages which are set automatically according to the actual intensity. Cell Detection 1100 Series FD Reference Manual...

  • Page 265: Flf Board Revisions

    There have been several board versions introduced since the introduction of the detector. Table 40 FLF Board revisions Part Revision Changes number G1321- original version. 66501 Raman ASTM signal to noise spec is >200 1100 Series FD Reference Manual 265...

  • Page 266: How To Retrieve The Flf Board Revision

    The FLF board revision can be retrieved with the following ChemStation command: PRINT SENDMODULE$(LFLD,"FLFR?") The reply will be: RA 0000 FLFR "AAAA" for revsion A boards. Control Module (G1323A/B) 1 Select FLD TESTS 2 Press m.m (m-dot-m) 3 Select Command 4 Type: FLFR? 1100 Series FD Reference Manual...

  • Page 267: Detector Lamp Supply Board (Fll)

    An ignition voltage is switched by a thyristor to the TriggerPac ignition transformer “Igniting the Flash Lamp” to built a small ionized channel (refer on page 270). A freewheeling diode forces the thyristor to switch off again to prevent lamp damage. 1100 Series FD Reference Manual 267...

  • Page 268: Firmware Description

    • a non-instrument specific section, called resident system, • an instrument specific section, called main system. Resident System This resident section of the firmware is identical for all Agilent 1100 series modules. Its properties are: • the complete communication capabilities (GPIB, CAN, LAN and RS-232C), •...

  • Page 269: Raw Data Conversion To Fluorescence (Lu) Units

    LU (light or luminescence units) is used as new unit and will indicate the light intensity (not comparable with the physical unit Lumen!). These units are calculated from the PMT (photomuliplier tube) in the emission path and a reference diode located behind the flow cell, see figure below. 1100 Series FD Reference Manual 269...
  • Page 270 Theory of Operation Figure 92 Optical Diagram of the FLD 1100 Series FD Reference Manual...

  • Page 271: Data Flow For Chromatographic Output

    Responsetime assigned for chromatographic Peak Detector output Output ( LU ) Figure 93 Data flow for chromatographic output For multi-channel output, any single flash data point will be processed in a separate independent filter. 1100 Series FD Reference Manual 271...

  • Page 272: Data Flow For Spectral Output

    Control Module ChemStation spectra LU Online Monitor Spline algorithm ( raw ) smoothed spectra output Data Analysis ( LU ) Figure 94 Data flow for spectral output Raw Signal Acquisition (PMT and Reference Diode) 1100 Series FD Reference Manual...
  • Page 273 A. As point of reference the mid-point of each spectra is used. Concentration correction is not done • If the cuvette is used, e.g. fluorescence scan. • If ‘all spectra without signal’ is used as spectra acquisition mode. 1100 Series FD Reference Manual 273...

  • Page 274: Spectra Acquisition Modes

    Optional Interface Boards The Agilent 1100 Series modules have one optional board slot that allows addition of an interface board to the modules. 1100 Series FD Reference Manual...

  • Page 275: Bcd Board

    “BCD Cables” “External Contact Cable” on page 230 and the external outputs, see page 234 to external devices. Table 43 Detailed connector layout (1100) Signal name BCD digit BCD 5 BCD 7 BCD 6 1100 Series FD Reference Manual 275...

  • Page 276: Lan Communication Interface Board

    G13XX-66520 (for G1315A, G1365A, G1314A, G1310A, G1311A, G1312A and G1313A) or newer and on all other 1100 modules. a DOS- ChemStation software revision A.06.01 or above. The following cards can be used with the Agilent 1100 modules. 1100 Series FD Reference Manual...

  • Page 277: Interfaces

    ) Twisted pair network cable (shielded, 7 m long) 5023-0202 ( for hub connections ) Interfaces The Agilent 1100 Series modules provide the following interfaces : Table 45 Agilent 1100 Series Interfaces Interface Type Pumps Autosampler...

  • Page 278: Analog Signal Output

    • Interface slot for specific interfacing (external contacts, BCD, LAN and so on). For identification and location of the connectors Figure 6 on page 24. Never use cables other than the ones supplied by Agilent Technologies to ensure WARNING Ca le proper functionality and compliance with safety or EMC regulations, see O er ie on page 218.

  • Page 279: Can Interface

    Remote Interface The APG remote connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features such as common shut down, prepare, and so on. Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements.
  • Page 280 232C connection, using the appropriate software. This connector can be activated by the configuration switch module next to the GPIB connector. The RS-232C is designed as DCE (Data Communication Equipment) with a 9- pin male SUB-D type connector. The pins are defined as follows : 1100 Series FD Reference Manual...
  • Page 281 DCD 1 1 DCD RX 2 2 RX TX 3 3 TX DTR 4 4 DTR GND 5 5 GND DSR 6 6 DSR DB9 DB9 DB9 Male Female Female Male Figure 96 RS-232 Cable 1100 Series FD Reference Manual 281...

  • Page 282: Setting The 8-Bit Configuration Switch

    Factory setting is shown for the fluorescence detector Figure 97 8- bit Configuration Switch Table 49 8- bit Configuration Switch Mode Select GPIB GPIB Address RS-232C Baud rate Data Parity Bits Reserved Reserved TEST/BOOT RSVD RSVD RSVD 1100 Series FD Reference Manual...

  • Page 283: Gpib Default Addresses

    0 0 0 1 1 0 1 1 Autosampler 0 0 0 1 1 1 0 0 0 0 0 1 1 1 0 1 where 0 means that the switch is down and 1 means that the switch is up. 1100 Series FD Reference Manual 283...

  • Page 284: Communication Settings For Rs-232C Communication

    Table 52 Baud Rate Settings Switches Baud Rate Switches Baud Rate 9600 9600 1200 14400 2400 19200 4800 38400 Table 53 Data Bit Settings Switch 6 Data Word Size 7 Bit Communication 8 Bit Communication 1100 Series FD Reference Manual...
  • Page 285 If you use the following switch settings and power the instrument up again, a forced cold start has been completed. Table 55 Forced Cold Start Settings Mode Select TEST/BOOT To return to normal operation, set switches back to your GPIB or RS 232 configuration settings. 1100 Series FD Reference Manual 285...

  • Page 286: Resident Settings

    The line voltage can vary in a range from 100 – 120 or 220 – 240 volts AC ± 10 % and needs no manual setting. 1100 Series FD Reference Manual...
  • Page 287 The following table gives the specifications of the main power supply. Table 57 Main Power Supply Specifications 1100 Series FD Reference Manual 287...
  • Page 288 + 36 V must not exceed 107 W. Output 2 + 36 V / 2.5 A (maximum) Output 3 + 5 V / 3 A Output 4 + 15 V / 0.3 A Output 5 - 15 V / 0.3 A 1100 Series FD Reference Manual...

  • Page 289: Introduction To The Control Module

    Agilent 1100 Series Fluorescence Detector Reference Manual Introduction to the Control Module Major keys on the Agilent 1100 Control Module Screens available from the Analysis screen Screens available from the System screen Screens available from the Records screen Diagnostics and Tests...

  • Page 290: Major Keys On The Agilent 1100 Control Module

    LC Module firmware revision 3.8x NOTE ase the o trol odule’s displa see s to e froze ha g-up due to a communication problem on the CAN bus, unplug the control module from the LC module and reconnect. 1100 Series FD Reference Manual...

  • Page 291: Screens Available From The Analysis Screen

    The m-key allows access to the context sensitive menu. Setup view leads you to add sections for additional Agilent 1100 modules. Restart re-boots the control module. In the Setup view, e.g. the diode array detector can be added to the view. 1100 Series FD Reference Manual 291...
  • Page 292 The m-key gives access to a context sensitive menu (e.g. when the cursor is positioned in the excitation window). With the Settings key you open a pull-down menu where you can select the FLD module. Settings 1100 Series FD Reference Manual...
  • Page 293 FLD firmware revisions A.03.6X and below. Selecting More and Settings pull down menu you can enter special FLD setpoints. The PMT-Test allows the automatic check for optimum signal/noise and dynamic range under current conditions in the flow cell. 1100 Series FD Reference Manual 293...
  • Page 294 Selecting More and Scan on the pull down menu you can enter setpoints for spectrum acquisition (Multi-Ex or Multi-Em). Selecting More and 3D-scan on the pull down menu you can enter setpoints for taking for the 3D-fluorescence scans. Data can only be displayed using the 3 D-Agilent ChemStation software. 1100 Series FD Reference Manual...
  • Page 295 With the F2 key (Timetable) you can list the timetable for the FLD. Press F7 key (Insert) to add entries or F6 key (Delete) to remove entries. Press the F7 key (Insert) to add timetable events. Use the F6 key (Done) to view the entered lines of the timetable. 1100 Series FD Reference Manual 295...
  • Page 296 The F6 key (Store) will restart acquisition of spectra and loads the spectrum into memory in the control module. Spectra are lost when a new analysis is started or when the Control Module is switched off. The F8 key (Eval) leads to the next screen below. 1100 Series FD Reference Manual...
  • Page 297 From Menu item 1 (Setup Multi WL) you can switch between Excitation and Emission spectra and choose simultaneous multi-wavelengths detection. From Menu item 2 (Setup Scan) you can set spectra acquisition parameter. Store spectra is only valid if an Agilent Chemstation is connected. 1100 Series FD Reference Manual 297...
  • Page 298 (see Reference Manual of the Control Module). With the F8 key (Cursor) you can cruise with the cursor through the spectrum. The F6 key (Print) starts printing of the spectrum. Press Esc key to return to previous screen. 1100 Series FD Reference Manual...
  • Page 299 With the F5 key (Runtimes) you can change the stop time and the post-run time. Press F5 key (Views) and select Status. Status This is an example if an Agilent 1100 FLD is configured stand-alone. 1100 Series FD Reference Manual 299...
  • Page 300 (maximum 3), press F6 key (Select). If more than one signal is configured (see next), use the 1-2-3 number key to switch between the signals. Press the m- key to open the context sensitive menu. 1100 Series FD Reference Manual...
  • Page 301 PC-Card and Instrument window. Use the UP/Down arrows to select the method. Use the F7/F8 keys (Copy) to enter available signals into the box for selected signals or vice versa. Press the m-key to open the context sensitive menu. 1100 Series FD Reference Manual 301...

  • Page 302: Screens Available From The System Screen

    Introduction to the Control Module Screens available from the System screen System screen Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. This screen shows the last activities in the system. 1100 Series FD Reference Manual...
  • Page 303 Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F2 key (Configure) to select the FLD. Here you define further special setpoints for the FLD operation. Use the F1 key (Interfaces) to access the interface settings (if required ). 1100 Series FD Reference Manual 303...
  • Page 304 Introduction to the Control Module 1100 Series FD Reference Manual...

  • Page 305: Screens Available From The Records Screen

    Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F4 key (Records) to select the FLD. Errors are reported either into the System Log (F2) or Error Log (F3). 1100 Series FD Reference Manual 305...
  • Page 306 EMF (Early Maintenance Feedback) Use the F1 key (EMF) to set EMF parameters. Choose menu item 1 (Setup limits) to select lamp-on level for the Xenon lamp at which you want to receive a warning. 1100 Series FD Reference Manual...
  • Page 307 Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F3 key (Records) to select the FLD. Use the F5 key (FW Update) to enter the Update section. Select the a file from the PCMCIA card (1321nnnn.DLB) and 1100 Series FD Reference Manual 307...

  • Page 308: Diagnostics And Tests

    Use the F3 key (Records) to select the FLD. Use the F4 key (Maint log) to view and edit the maintenance logbook. Use the F7 key (Add) to add new maintenance activities. Diagnostics and Tests Tests screen 1100 Series FD Reference Manual...
  • Page 309 Menu item 3 (Schematics) will popup the FLD diagram. Lamp Characteristic Use the F5 key (Lamp Char) to get the instrument profile. Use F8 key (Take) to generate a new profile. 1100 Series FD Reference Manual 309...
  • Page 310 Use the F6 key (Plot) to view the signal. A simulated chromatogram (4 peaks) will repeat until the run is stopped. The signal is also available on the analog output. A change of the peakwidth will change the retention times. 1100 Series FD Reference Manual...
  • Page 311 Introduction to the Control Module 1100 Series FD Reference Manual 311...
  • Page 312 Introduction to the Control Module 1100 Series FD Reference Manual...

  • Page 313: Specifications

    Agilent 1100 Series Fluorescence Detector Reference Manual Specifications Performance Specifications...

  • Page 314: Performance Specifications

    Agilent Technologies Specifications Performance Specifications Table 59 Performance Specifications Agilent 1100 Series Fluorescence Detector Type Specification Comments Detection type Multi-signal fluorescence detector with rapid on-line scanning capabilities spectral data analysis Performance 10 fg Anthracene, see note below this table Specifications...
  • Page 315 4 signal wavelengths, programing: response time, PMT Gain, baseline behavior (append, free, zero), spectral parameters Specifications Table 59 Performance Specifications Agilent 1100 Series Fluorescence Detector, Type Specification Comments Spectrum acquisition: Excitation or Emission spectra Scan speed: 28 ms per datapoint (e.g.
  • Page 316 ChemStation), leak detection, safe leak handling, leak output signal for shutdown of pumping system. Low voltages in major maintenance areas. 1100 Series FD Reference Manual Specifications Table 59 Performance Specifications Agilent 1100 Series Fluorescence Detector, Type Specification Comments GLP features Early maintenance...
  • Page 317 Reference conditions: standard cell 8 µl, response time 4 s, flow 0.4 ml/min LC- NOTE grade Methanol, 2.1 x 100 mm ODS column. Agilent 1100 Series Fluorescence Detector Reference Manual Safety Information General Safety Information Lithium Batteries Information Radio Interference...
  • Page 318 Agilent Technologies 1100 Series FD Reference Manual...

  • Page 319: General Safety Information

    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 320 Table 60 Safety Symbols Symbol Description The apparatus is marked with this symb ol when the user should refer to the instruction manual in order to pr otect the apparatus against damage. Indicates dangerous voltages. 1100 Series FD Reference Manual...

  • Page 321: Lithium Batteries Information

    Lithium Batteries Information WARNING Danger of explosion if battery is incorrectly replaced. Replace only with the same or equivalent type recommended by the equipment manufacturer. Lithium batteries may not be disposed-off into the domestic waste. 1100 Series FD Reference Manual 321...
  • Page 322 Eksplosionsfare. Ved udskiftning benyttes kun batteri som anbefalt WARNING av apparatfabrikanten. Brukt batteri returneres WARNING appararleverandoren. Bij dit apparaat zijn batterijen geleverd. Wanneer deze leeg zijn, moet u ze niet NOTE weggooien maar inleveren als KCA. 1100 Series FD Reference Manual...

  • Page 323: Radio Interference

    Safety Information 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 If test and measurement equipment is operated with equipment unscreened cables and/or used for measurements on open set-ups, the user has to assure that under operating conditions the radio interference limits are still met within the premises.

  • Page 324: Sound Emission

    This product has a sound pressure emission (at the operator position) < 70 dB. • Sound Pressure Lp < 70 dB ( A ) • At Operator Position • Normal Operation • According to ISO 7779:1988/EN 27779/1991 (Type Test) 1100 Series FD Reference Manual...

  • Page 325: Uv-Radiation (Uv-Lamps Only)

    Table 62 UV-Radiation Typical Values Position Effective Irradiance Lamp installed, 50-cm distance average 0.016 µW/cm Lamp installed, 50-cm distance maximum 0.14 µW/cm Solvent Information Observe the following recommendations on the use of solvents. Flow Cell 1100 Series FD Reference Manual 325...
  • Page 326 For example, a 1-% solution of acetic acid in methanol will attack steel. • Solutions containing strong complexing agents (for example, EDTA, ethylene diamine tetra-acetic acid). • Mixtures of carbon tetrachloride with 2-propanol or THF. 1100 Series FD Reference Manual...
  • Page 327 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” It will provide also the latest firmware of the Agilent 1100 series modules for download. 1100 Series FD Reference Manual 327...

  • Page 328: A Safety Information

    Safety Information 1100 Series FD Reference Manual...
  • Page 329 EMF (early switch description, main maintenance feedback), default settings, description system, raw data emission condenser, and factory settings, control conversion, emission grating, module resident system, emission Analysis screens, updates, 200, monochromator, 1100 Series FD Reference Manual 329...
  • Page 330 1100 Series FD Reference Manual...
  • Page 331 (BCD/LAN), resistance reference system, removing DAC, monochromators, covers, 146, repair dark current, responsetime, functions, flushing of flow cell, RS-232C cable kit to PC, lamp Repairing, repairs communication intensity, Index 1100 Series FD Reference Manual 331...
  • Page 332 78, no peaks, status indicators, 78, unpacking, using EMF, UV degradation, 119, wavelength recalibration, 78, wavelength calibration, wavelength calibration procedure, 105, wavelength calibration steps, wavelength shift of spectra, weight and dimensions, xenon flash lamp, 243, 1100 Series FD Reference Manual...
  • Page 334 In This Book This manual contains technical reference information about the Agilent 1100 Series fluorescence detector. The manual describes the following: • installing the detector, • optimization of the detector, • diagnostics and troubleshooting, • repairing the detector, • parts and materials, and •...

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