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In This Manual… This manual contains information for using your Diode Array and Multiple Wavelength Detectors. Introduction to the Detector This chapter gives an introduction to the detector, instrument overview and internal connectors. Site Requirements and Specifications This chapter gives information on environmental requirements, physical and performance specifications.
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Parts and Materials for Maintenance This chapter provides information on parts for maintenance. Appendix This chapter provides safetey and other general information. 1200 Series DAD and MWD User Manual...
Contents Introduction to the Detector Introduction to the Detector Optical System Overview Early Maintenance Feedback (EMF) EMF Counters Using the EMF Counters Electrical Connections Instrument Layout Site Requirements and Specifications Site Requirements Physical Specifications Performance Specifications Installing the Detector Unpacking the Detector Damaged Packaging Delivery Checklist Optimizing the Stack Configuration...
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Before Using the System Requirements and Conditions Optimization of the System Preparing the HPLC System Running the Sample and Verifying the Results Special Settings of the Detector Control Settings Online Spectra Analog Output Settings Spectrum Settings Peakwidth Settings Slit Settings Margin for Negative Absorbance Settings Optimizing the Detector How to optimize the Detector...
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Troubleshooting and Diagnostics Overview of the Detector’s Indicators and Test Functions Status Indicators Power Supply Indicator Detector Status Indicator User Interfaces Agilent LC Diagnostic Software Maintenance and Repair Introduction into Repairing the Detector Simple Repairs Exchanging Internal Parts Warnings and Cautions Cleaning the Detector Using the ESD Strap Maintenance...
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Correcting Leaks Replacing Leak Handling System Parts Replacing the Interface Board Replacing the Detector’s Firmware Tests & Calibrations Intensity Test Wavelength Verification and Recalibration Holmium Oxide Test Cell Test (ChemStation only) Parts and Materials for Maintenance Overview of Maintenance Parts Standard Flow Cell Semi-Micro Flow Cell Micro Flow Cell...
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Sound Emission UV-Radiation Solvent Information Declaration of Conformity for HOX2 Filter Agilent Technologies on Internet Index 1200 Series DAD and MWD User Manual...
Agilent 1200 Series Diode Array and Multiple Wavelength Detectors User Manual Introduction to the Detector Introduction to the Detector Optical System Overview Early Maintenance Feedback (EMF) Electrical Connections Instrument Layout This chapter gives an introduction to the detector, instrument overview and internal connectors. Agilent Technologies...
• easy front access to lamps and flow cell for fast replacement, and • built-in holmium oxide filter for fast wavelength accuracy verification, • built-in temperature control for improved baseline stability (G1315B DAD and G1365B MWD). For specifications, see “Performance Specifications”...
Introduction to the Detector Optical System Overview Optical System The optical system of the detector is shown in Figure 1. Its illumination source is a combination of a deuterium-arc-discharge lamp for the ultraviolet (UV) wavelength range and a tungsten lamp for the visible (VIS) and short-wave near-infrared (SWNIR) wavelength range.
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Introduction to the Detector wavelength range. The light source for the visible and SWNIR wavelength range is a low noise tungsten lamp. This lamp emits light over the wavelength range 470 – 950 nm. Achromat The achromat receives the light from both lamps and focuses it so that the (Source Lens) beam passes through the flow cell.
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Introduction to the Detector Diode Array The diode array is a series of 1024 individual photodiodes and control circuits located on a ceramic carrier. With a wavelength range from 190 – 950 nm the sampling interval is < 1 nm. 1200 Series DAD and MWD User Manual...
Introduction to the Detector Early Maintenance Feedback (EMF) Maintenance requires the exchange of components which are subject to wear or stress. Ideally, the frequency at which components are exchanged should be based on the intensity of usage of the detector and the analytical conditions, and not on a predefined time interval.
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Introduction to the Detector Setting the EMF Limits The setting of the EMF limits must be optimized over one or two maintenance cycles. Initially, no EMF limit should be set. When instrument performance indicates maintenance is necessary, take note of the values displayed by lamp counters.
Introduction to the Detector Electrical Connections • The GPIB connector is used to connect the detector with a computer. The address and control switch module next to the GPIB connector determines the GPIB address of your detector. The switches are preset to a default address which is recognized once after power is switched on.
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Introduction to the Detector Security lever Interface board Analog signals APG remote RS-232C GPIB Power serial number: manufactured in Germany Configuration switch 2006 week of last major change 00130 number of unit product number serial number safety standards configuration switch settings voltage range power consumption /...
Introduction to the Detector Instrument Layout The industrial design of the detector incorporates several innovative features. It uses Agilent’s E-PAC concept for the packaging of electronics and mechanical assemblies. This concept is based upon the use of expanded polypropylene (EPP) layers of foam plastic spacers in which the mechanical and electronic boards components of the detector are placed.
Agilent 1200 Series Diode Array and Multiple Wavelength Detectors User Manual Site Requirements and Specifications Site Requirements Physical Specifications Performance Specifications This chapter gives information on environmental requirements, physical and performance specifications. Agilent Technologies...
Site Requirements and Specifications 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. Consequently, there is no voltage selector in the rear of the detector.
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Never operate your instrumentation from a power outlet that has no ground WA R N I N G connection. Never use a power cord other than the Agilent Technologies power cord designed for your region. Never use cables other than the ones supplied by Agilent Technologies to ensure WA R N I N G proper functionality and compliance with safety or EMC regulations.
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Site Requirements and Specifications The G1315B DAD and G1365B MWD are designed to operate in a typical electromagnetic N O T E environment (EN61326-1) where RF transmitters, such as mobile phones, should not be used in close proximity. 1200 Series DAD and MWD User Manual...
Line voltage 100 – 240 VAC, 10 % Wide-ranging capability ± Line frequency 50 or 60 Hz Power consumption (G1315B/65B) 300 VA / 125 W / 427 BTU Maximum ° ° Ambient operating temperature 0 – 55 C (32 – 131 °...
Site Requirements and Specifications Performance Specifications Table 2 Performance Specifications Agilent 1200 Series DAD and MWD Type Specification Comments Detection type 1024-element photodiode array Light source Deuterium and tungsten lamps Wavelength range 190 – 950 nm Short term noise (ASTM) ±...
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Site Requirements and Specifications Table 2 Performance Specifications Agilent 1200 Series DAD and MWD, continued Type Specification Comments Communications Controller-area network (CAN), GPIB, RS-232C, APG Remote: ready, start, stop and shut-down signals, LAN optional Safety and maintenance Extensive diagnostics, error detection and display (through control module and ChemStation), leak detection, safe leak handling, leak output signal for shutdown of pumping system.
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Site Requirements and Specifications 1200 Series DAD and MWD User Manual...
Agilent 1200 Series Diode Array and Multiple Wavelength Detectors User Manual Installing the Detector Unpacking the Detector Optimizing the Stack Configuration Installing the Detector Flow Connections to the Detector This chapter describes the installation of the detector. Agilent Technologies...
Damaged Packaging If the delivery packaging shows signs of external damage, please call your Agilent Technologies sales and service office immediately. Inform your service representative that the detector may have been damaged during shipment. If there are signs of damage, please do not attempt to install the detector.
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Installing the Detector Detector Accessory Kit Contents Table 4 Accessory Kit Contents Description Part Number Quantity Accessory kit G1315-68705 CAN cable 0.5 m 5181-1516 Teflon Tubing flexible i.d. 0.8 mm (flow cell to waste), 5062-2462 re-order 5 m Corrugated tubing (to waste), re-order 5 m 5062-2463 1.2 m Fitting male PEEK...
Installing the Detector Optimizing the Stack Configuration If your detector is part of a complete Agilent 1200 Series system, you can ensure optimum performance by installing the following configuration. This configuration optimizes the system flow path, ensuring minimum delay volume. 1200 Series DAD and MWD User Manual...
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Installing the Detector Solvent cabinet Vacuum degasser Local User Pump Interface Autosampler Column compartment Detector Figure 3 Recommended Stack Configuration (Front View) 1200 Series DAD and MWD User Manual...
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Installing the Detector Remote cable CAN Bus cable to local user interface CAN Bus cable AC power Analog detector signal (1 or 2 outputs per detector) LAN to LC ChemStation (location depends on detector) Figure 4 Recommended Stack Configuration (Rear View) 1200 Series DAD and MWD User Manual...
Installing the Detector Installing the Detector Preparations Locate bench space Provide power connections Unpack the detector Parts required Detector Power cord, for other cables see below ChemStation and/or Control Module G1323B or Instant Pilot G4208A 1 Install the LAN interface board in the detector (if required), see “Replacing the Interface Board”...
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Installing the Detector 4 Connect the power cable to the power connector at the rear of the detector. 5 Connect the CAN cable to other Agilent 1200 Series modules. 6 If a Agilent ChemStation is the controller, connect the LAN connection to the LAN interface board in the detector.
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Installing the Detector The detector is turned on when the line power switch is pressed and the green indicator N O T E lamp is illuminated. The detector is turned off when the line power switch is protruding and the green light is OFF. To disconnect the detector from line, unplug the power cord.
Installing the Detector Flow Connections to the Detector Preparations Detector is installed in the LC system. Parts required Other modules Parts from accessory kit, see“Detector Accessory Kit Contents” on page 31. Two wrenches 1/4 – 5/16 inch for capillary connections When working with solvents please observe appropriate safety procedures (for WA R N I N G example, goggles, safety gloves and protective clothing) as described in the...
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Installing the Detector 1 Press the release buttons and remove the front cover to 2 Press the release button and open the flow cell door. gain access to the flow cell area. 3 Insert the flow cell and install the capillaries to the 4 If another Agilent 1200 Series module is positioned on top capillary holder (top is inlet, bottom is outlet).
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Installing the Detector 5 Assemble the column-detector capillary from the 6 Connect the newly assembled fitting of the capillary to the accessory kit. One side is already factory-assembled top fitting holder and the other end to the column. Pre-assembled 7 Assemble the waste tubing from the accessory kit. 8 Connect the waste tubing to the bottom fitting holder and a waste tubing to the leak outlet.
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Installing the Detector 9 Remove the flow cell and establish a flow and observe for 10 Insert the flow cell, close the cover and replace the front leaks. cover. The installation of the detector is now complete. The detector should be operated with the front cover in place to protect the flow cell area N O T E against strong drafts from the ouside and to cover the deuterium lamp.
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Installing the Detector 1200 Series DAD and MWD User Manual...
Online Spectra Analog Output Settings Spectrum Settings Peakwidth Settings Slit Settings Margin for Negative Absorbance Settings Optimizing the Detector This chapter provides information on how to set up the detector for an analysis and explains the basic settings. Agilent Technologies...
Using the Detector Setting up an Analysis This chapter can be used for • preparing the system, • to learn the set up of an HPLC analysis and • to use it as an instrument check to demonstrate that all modules of the system are correctly installed and connected.
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Using the Detector Table 5 Choice of Priming Solvents for Different Purposes Activity Solvent Comments After an installation Isopropanol Best solvent to flush air out of the system When switching between reverse Isopropanol phase and normal phase (both times) Best solvent to flush air out of the system After an installation Ethanol or Methanol...
Using the Detector Requirements and Conditions What You Will Need Table 6 lists the items you need to have for the set up of the analysis. Some of these are optional (not required for the basic system). Table 6 What you will need 1200 system Pump (plus degassing) Autosampler...
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Using the Detector Conditions A single injection of the isocratic test standard is made under the conditions given in Table 7: Table 7 Conditions Flow 1.5 ml/minute Stoptime 8 minutes Solvent 100% (30% water/70% Acetonitrile) Temperature Ambient Wavelength sample 254 nm (4 nm bandwidth) reference 360 nm (100 nm bandwidth) Injection Volume 1 µl...
Using the Detector Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 7. The exact profile of the chromatogram will depend on the chromatographic conditions. Variations in solvent quality, column packing, standard concentration and column temperature will all have a potential effect on peak retention and response.
Using the Detector Preparing the HPLC System 1 Turn on the Agilent ChemStation PC and the monitor. 2 Turn on the 1200 series HPLC modules. 3 Start the Agilent ChemStation software (B.02.01). If the pump, autosampler, thermostatted column compartment and detector are found, the ChemStation screen should look like shown in Figure The System status is red (Not Ready).
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Using the Detector 4 Turn on the detector lamp, pump and autosampler by clicking the System On button or the buttons below the module icons on the graphical user interface (GUI). After some time, the pump, thermostatted column compartment and detector module will turn to green. Figure 9 Turning on the HPLC Module 1200 Series DAD and MWD User Manual...
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Using the Detector 5 Purge the pump. For more information see “Priming and Purging the System” on page 44. 6 Allow the detector to warm up of at least 60 minutes to provide a stable baseline (see example in Figure 10 Table For reproducible chromatography, the detector and lamp should be on for at least one hour.
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Using the Detector 7 For the isocratic pump, fill the solvent bottle with the mixture of HPLC-grade bi-distilled water (30 %) and acetonitrile (70 %). For binary- and quaternary pumps you can use separate bottles. 8 Click on the Load Method button and select and press OK.
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Using the Detector 9 Click on the module icons (Figure 12) and open the Setup of these modules. Figure 13 on page 54 shows the detector settings (do not change the detector parameters at this time). Figure 12 Open the module menu 10 Enter the pump parameters mentioned under “Conditions”...
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Using the Detector • up to 5 signals (A to E) with individual wavelength settings can be selected. • spectrum settings, see page • stop and post time can be set (if required) • depending on the application, the lamps can be selected (one or both).
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Using the Detector 11 Pump the water/acetonitrile (30/70 %) mobile phase through the column for 10 minutes for equilibration. 12 Click the button and select Change... to open the Signal Plot information. Select the Pump: Pressure and the DAD A: Signal 254,4 as signals.
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Using the Detector The Online Plot (Figure 15 on page 56) shows both, the pump pressure and the detector absorbance signals. Pressing Adjust the signals can be reset to the offset value and Balance would do a balance on the detector. Pump pressure signal DAD absorbance signal Figure 15...
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Using the Detector 14 Select the menu item RunControl -> Sample Info and enter information about this application (Figure 16 on page 57). Press OK to leave this screen. Figure 16 Sample Information 15 Fill the content of an isocratic standard sample ampoule into a vial and seal the vial with a cap and place the vial into autosampler tray (position #1).
Using the Detector Running the Sample and Verifying the Results 1 To start a run select the menu item RunControl -> Run Method. 2 This will start the 1200 modules and the online plot on the Agilent ChemStation will show the resulting chromatogram. Figure 17 Chromatogram with Isocratic Test Sample Information about using the Data Analysis functions can be obtained from the Using your...
Using the Detector Special Settings of the Detector In this chapter special settings of the G1315B DAD and G1365B MWD are described (based on the Agilent ChemStation B.02.01). Control Settings • Lamps: turn on and off of UV- and Vis lamp.
Using the Detector Online Spectra 1 To view the online spectra during the run select Online Spectra. Figure 19 Online Spectra Window 2 Change the absorbance and wavelength range according your needs. 1200 Series DAD and MWD User Manual...
Using the Detector Analog Output Settings To change the Output Range of the analog outputs see “Control Settings” page 59. 1 To change the offset and the attenuation select Analog Outputs. 2 Change the ranges for absorbance and wavelength according your needs. Zero Offset Limits: 1 to 99% in steps of 1% Attenuation Limits: 0.98 to 2000 mAU at discrete values for either 100 mV or 1 V full...
Using the Detector Spectrum Settings To change the Spectra settings open. 1 To change the Spectra settings select Setup Detector Signals. 2 In the section Spectrum click on the drop-down list and chose a parameter. Table 9 on page 63 shows the possible parameters. 3 Change the Range, Step width and Threshold according to your needs.
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Using the Detector Table 9 Spectrum Settings Store Defines at which points on “signal A” spectra will be taken and saved. Signal A is used to control the “peak controlled spectra acquisition”; the other signals have no influence on spectra acquisition. None No spectra are taken.
Using the Detector Peakwidth Settings • Do not use peak width shorter than necessary N O T E 1 To change the Peakwidth settings select Setup Detector Signals. 2 In the section Peakwidth (Responsetime) click on the drop-down list. 3 Change the Peakwidth according to your needs. Peakwidth enables you to select the peak width (response time) for your analysis.
Using the Detector Table 10 Peak Width — Response Time — Data Rate Peak Width (min) Response Time (sec) Data Rate (Hz) <0.01 >0.01 >0.03 >0.05 >0.10 >0.20 1.25 >0.40 0.62 >0.85 16.0 0.31 Slit Settings 1 To change the Slit settings select Setup Detector Signals. 2 In the section Slit click on the drop-down list.
Using the Detector Margin for Negative Absorbance Settings 1 To change the settings select Setup Detector Signals. 2 In the section Margin for Negative Absorbance change the value according to your needs. Use this field to modify the detector’s signal handling to increase the margin for negative absorbance.
Agilent 1200 Series Diode Array and Multiple Wavelength Detectors User Manual How to optimize the Detector Optimizing the Detector Performance Optimization Overview Optimizing for Sensitivity, Selectivity, Linearity and Dispersion Optimizing Selectivity This chapter provides information on how to optimize the detector. Agilent Technologies...
How to optimize the Detector Optimizing the Detector Performance The detector has a variety of parameters that can be used to optimize performance. Depending on whether signal or spectral data need to be optimized, different settings are recommended. The following sections describe optimization for: •...
How to optimize the Detector Optimization Overview Table 11 Optimization Overview Parameter Impact 1 Selection of flow cell • peak resolution versus sensitivity • Choose flow cell according to used column, see Figure 2 Connection of flow cell • chromatographic resolution •...
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How to optimize the Detector Table 11 Optimization Overview, continued Parameter Impact 5 Setting the slit width • Use 4 nm slit for normal applications. • spectral resolution, sensitivity and • Use narrow slit (e.g 1 nm) if your analytes have narrow absorbance linearity.
How to optimize the Detector Optimizing for Sensitivity, Selectivity, Linearity and Dispersion Flow Cell Path Length Lambert-Beer’s law shows a linear relationship between the flow cell path length and absorbance. ε ⋅ ⋅ Absorbance --- - – where T is the transmission, defined as the quotient of the intensity of the transmitted light I divided by the intensity of the incident light, I ε...
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How to optimize the Detector Analysis of pesticide standard 6-mm optical path length 10-mm optical path length Time (min) Figure 26 Influence of Cell Path Length on Signal Height Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards. To check photometric accuracy of the Agilent 1200 DAD/MWD it is necessary to have more precise information on path lengths of the flow cells.
How to optimize the Detector Peak width (response time) Response time describes how fast the detector signal follows a sudden change of absorbance in the flow cell. The detector uses digital filters to adapt response time to the width of the peaks in your chromatogram. These filters do not affect peak area nor peak symmetry.
How to optimize the Detector Table 13 Peak Width — Response Time — Data Rate Peak Width [minutes] Response Time [seconds] Data Rate [Hz] <0.01 >0.01 >0.03 >0.05 >0.10 >0.20 1.25 >0.40 0.62 >0.85 16.0 0.31 Sample and Reference Wavelength and Bandwidth The detector measures absorbance simultaneously at wavelengths from 190 to 950 nm.
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How to optimize the Detector The signals comprises a series of data points over time, with the average absorbance in the sample wavelength band minus the average absorbance of the reference wavelength band. Signal A in the detector default method is set to sample 250,100, reference 360,100, that is, the average absorbance from 200 –...
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How to optimize the Detector A wide bandwidth has the advantage of reducing noise by averaging over a wavelength range — compared to a 4 nm bandwidth, the baseline noise is reduced by a factor of approximately 2.5, whereas the signal is about 75 % of a 4-nm wide band.
How to optimize the Detector 1 pmol each Wavelength 267 nm Reference 380 nm Wavelength 267 nm No reference Time (min) Grad.: 0.02 m KH /ACN from 12% ACN to 45% ACN in 12 min Figure 30 Gradient Analysis of PTH-Amino Acids (1 pmol each), with and without Refer- ence Slit Width The detector has a variable slit at the entrance of the spectrograph.
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How to optimize the Detector 16 nm 4 nm 1 nm Figure 31 Benzene at 1, 4 and 16 nm slit width A wide slit uses more of the light shining through the flow cell. This gives lower baseline noise as shown in Figure Slit width 1 nm Slit width 4 nm...
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How to optimize the Detector Furthermore, the absorbance is no longer strictly linear with concentration for wavelengths at a steep slope of a compound’s spectrum. Substances with fine structures and steep slopes like benzene are very rare. In most cases the width of absorbance bands in the spectrum is more like 30 nm as with anisic acid (see Figure 28).
How to optimize the Detector Optimizing Spectral Acquisition (DAD only) Storage of all spectra consumes a lot of disk space. It is very useful to have all spectra available during optimization of a method or when analyzing unique samples. However when running many samples of the same type, the large size of data files with all spectra may become a burden.
How to optimize the Detector Margin for Negative Absorbance The detector adjusts its gain during balance such that the baseline may drift slightly negative (about -100 mAU). In some special case, for example, when gradient with absorbing solvents are used, the baseline may drift to more negative values.
How to optimize the Detector Optimizing Selectivity Quantifying Coeluting Peaks by Peak Suppression In chromatography, two compounds may often elute together. A conventional dual-signal detector can only detect and quantify both compounds independently from each other if their spectra do not overlap. However, in most cases this is highly unlikely.
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How to optimize the Detector WL1 (204 nm, caffeine) WL2 (222 nm, hydrochlorothiazide WL3 (260 nm, reference to suppress hydrochlorothiazide WL4 (282 nm, reference to suppress caffeine Wavelength (nm) Figure 33 Wavelength Selection for Peak Suppression With a UV-visible detector based on a diode array and the correct choice of a reference wavelength setting, quantitative detection is possible.
How to optimize the Detector Hydrochlorothiazide Hydrochlorothiazide and caffeine and caffeine Wavelength 204 nm Wavelength 222 nm No reference No reference Caffeine suppressed Hydrochlorothiazide suppressed Wavelength 222 nm Wavelength 204 nm Reference 282 nm Reference 260 nm Time (min) Time (min) Figure 34 Peak Suppression Using Reference Wavelength Ratio Qualifiers for Selective Detection of Compound Classes...
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How to optimize the Detector Select 2 characteristic wavelengths Signal = WL1/WL2 20% o-Terphenyl Biphenyl Wavelength (nm) Figure 35 Wavelength Selection for Ratio Qualifiers Signals at 250 nm Biphenyl o-Terphenyl No selectivity With ratio qualifier 250/222 nm = 3.5 Time (min) Figure 36 Selectivity by Ratio Qualifiers In a four-component mixture, only biphenyl was recorded.
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How to optimize the Detector ± The ratio range was set at 2 – 2.4 (2.2 10%). Only when the ratio between 249 and 224 nm was within this range, is the signal plotted. Of all four peaks, only the third fulfilled the criterion (Figure 36).
Troubleshooting and Diagnostics Overview of the Detector’s Indicators and Test Functions 88 Status Indicators 89 User Interfaces 91 Agilent LC Diagnostic Software 92 This chapter gives an overview about the troubleshooting and diagnostic features and the different user interfaces. Agilent Technologies...
Troubleshooting and Diagnostics Overview of the Detector’s Indicators and Test Functions Status Indicators The detector is provided with two status indicators which indicate the operational state (prerun, run, and error states) of the detector. The status indicators provide a quick visual check of the operation of the detector (see page 51).
Troubleshooting and Diagnostics 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. Status indicator green/yellow/red Line power switch with green light Figure 37 Location of Status Indicators Power Supply Indicator...
Troubleshooting and Diagnostics Detector Status Indicator The detector status indicator indicates one of four possible detector conditions: • When the status indicator is OFF (and power switch light is on), the detector is in a prerun condition, and is ready to begin an analysis. •...
Troubleshooting and Diagnostics User Interfaces Depending on the user interface the available tests vary. All test descriptions are based on the Agilent ChemStation as user interface. Some descriptions are only available in the Service Manual. Table 14 Test Functions avaible vs. User Interface Test ChemStation Instant Pilot...
Troubleshooting and Diagnostics Agilent LC Diagnostic Software The Agilent LC diagnostic software is an application independent tool that provides troubleshooting capabilities for the Agilent 1200 Series modules. It provides for all 1200 Series LC the possibility of a first guided diagnostic for typical HPLC symptoms and a status report stored as Adobe Acrobat pdf or as a printable file to assist users evaluating the instrument state.
Agilent 1200 Series Diode Array and Multiple Wavelength Detectors User Manual Maintenance and Repair Introduction into Repairing the Detector Warnings and Cautions Cleaning the Detector Using the ESD Strap This chapter provides general information on maintenance and repair of the detector. Agilent Technologies...
Maintenance and Repair Introduction into Repairing the Detector Simple Repairs The detector is designed for easy repair. The most frequent repairs such as lamp change and flow cell change can be done from the front of the detector with the detector in place in the system stack. These repairs are described in “Maintenance”...
Maintenance and Repair Warnings and Cautions To prevent personal injury, the power cable must be removed from the instrument WA R N I N G before opening the detector cover. Do not connect the power cable to the detector while the covers are removed. To prevent personal injury, be careful when getting in contact with sharp metal WA R N I N G areas.
Maintenance and Repair Cleaning the Detector The detector case should be kept clean. Cleaning should be done with a soft cloth slightly dampened with water or a solution of water and mild detergent. Do not use an excessively damp cloth allowing liquid to drip into the detector. Do not let liquid drip into the detector.
Maintenance and Repair Using the ESD Strap Electronic boards are sensitive to electronic discharge (ESD). In order to prevent damage, always use an ESD strap when handling electronic boards and components. 1 Unwrap the first two folds of the band and wrap the exposed adhesive side firmly around your wrist.
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Maintenance and Repair 1200 Series DAD and MWD User Manual...
Replacing Leak Handling System Parts Replacing the Interface Board Replacing the Detector’s Firmware Tests & Calibrations Intensity Test Wavelength Verification and Recalibration Holmium Oxide Test Cell Test (ChemStation only) This chapter describes the maintenance of the detector and the required tests. Agilent Technologies...
Maintenance Overview of Maintenance The following pages describe maintenance (simple repairs) of the detector that can be carried out without opening the main cover. Table 15 Simple Repairs Procedure Typical Frequency Notes Deuterium lamp or If noise and/or drift exceeds your application limits or An intensity test should be performed tungsten lamp lamp does not ignite.
Maintenance Exchanging a Lamp When required If noise or drift exceeds application limits or lamp does not ignite Tools required Screwdriver POZI 1 PT3 Parts required Longlife Deuterium lamp 2140-0813 (without black cover) Longlife Deuterium lamp 5181-1530 (with black cover) Tungsten lamp G1103-60001 Preparations Turn the lamp(s) off.
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Maintenance 3 When replacing the vis-lamp, assure that the vis-lamp is 4 Insert the lamp. Fix the screws and reconnect the lamp to inserted as shown (flat edge towards the deuterium lamp connector. - opposite as in the figure). 6 Replace the front cover. Next steps: 7 Reset the lamp counter as described in the user interface documentation.
Maintenance Exchanging a Flow Cell When required If an application needs a different type of flow cell or the flow cell needs repair. Tools required Two 1/4 inch wrenches for capillary connections Parts required Standard flow cell, 10 mm, 13 µl, 120 bar, G1315-60022 Semi-micro flow cell, 6 mm, 5 µl, 120 bar, G1315-60025 Micro flow cell, 3 mm, 2 µl, 120 bar, G1315-60024 High pressure flow cell, 6 mm, 1.7 µl, 400 bar, G1315-60015...
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Maintenance Note: 3 Disconnect the cell inlet and the cell outlet capillary and the waste capillary from the capillary holder. Depending on the system setup, the inlet capillary might be routed directly from the module above or below to the cell and not to the capillary holder. 4 Loosen the thumb screw and remove the flow cell outlet 5 Remove the flow cell while pressing the flow cell holder.
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Maintenance Note: 6 Insert the flow cell while pressing the flow cell holder. The label attached to the flow cell provides information on part number, path length, volume and maximum pressure. If you want to replace flow cell parts, see “Maintenance of Standard, Semi-Micro or Micro Flow Cell”...
Maintenance Maintenance of Standard, Semi-Micro or Micro Flow Cell When required If the flow cell needs repair due to leaks or contaminations (reduced light throughput) Tools required Two 1/4 inch wrenches for capillary connections hexagonal key 4 mm Tooth picks Parts required For parts, see “Standard Flow Cell”...
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Maintenance Note: Use a 4 mm hex key to unscrew the window assembly and remove the gasket from the cell body. If you want to replace the gasket only, continue with step 7. Do not mix the gasket #6 and # 7. They are different for standard and semi-mirco flow cell.
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Maintenance Orientation of Flow Cell Parts NOTE Gaskets # 6 and #7 have different hole diameters 1 - window screw 2 - spring washers 3 - compression washer 4 - window holder 5 - quartz window 6 - gasket (light in) 7 - gasket (light out) 8 - window screw (contains items 2, 3, 4 and 5)
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Maintenance Press the Teflon® ring into the window assembly. Press the window assembly onto the new or cleaned quartz window. Insert a new gasket [6, 7] and the window assembly Using a 4-mm hex key, tighten the window screw hand into the cell body.
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Maintenance Next steps: 10 Reconnect the capillaries, see “Exchanging a Flow Cell” on page 103. 11 Perform a leak test. 12 Insert the flow cell. 13 Replace the front cover 14 Perform a “Wavelength Verification and Recalibration” on page 138 or a “Holmium Oxide Test”...
Maintenance Maintenance of High Pressure Flow Cell When required If the flow cell needs repair due to leaks or contaminations (reduced light throughput) Tools required Two 1/4 inch wrenches for capillary connections hexagonal key 4 mm Tooth picks Parts required For parts see “High Pressure Flow Cell”...
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Maintenance If you want to replace the gasket only, continue with Use a 4 mm hex key to unscrew the window assembly [1] step 7 on page 109. and remove the gasket [2] from the cell body. Note: Use a tooth pick to remove the quartz window from the window assembly.
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Maintenance Orientation of Flow Cell Parts 1 - window assembly (contains items 2, 3, 4, 5 and 6 2 - seal ring 3 - quartz window 4 - compression washer 5 - spring washers 4 - window holder 6 - window screw 7 - inlet capillary 8 - outlet capillary on page 106...
Maintenance Replacing Capillaries on a Standard Flow Cell When required If the capillary is blocked Tools required Two 1/4 inch wrenches for capillary connections Wrench 4 mm for capillary connections Screwdriver Pozi 1 PT3 Parts required For parts see “Standard Flow Cell” on page 146 Preparations Turn the lamp(s) off.
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Maintenance Identify the inlet and outlet capillaries. To replace the inlet After replacing the outlet capillary, fix it handtight first. capillary, continue with step 3. Then do a 1/4 turn with a 4-mm wrench. Inlet Outlet Outlet To replace the inlet capillary, use a 4-mm wrench for the Unscrew the cell body from the heat exchanger and the fitting.
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Maintenance Use a small flat screw driver to carefully lift off the I.D. tag. Unscrew the fixing screw and unwrap the inlet capillary Shown is the default orientation. See Note on page 114. from the grove in the flow cell body. Screw Inlet capillary with heat...
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Maintenance Insert the capillary into the hole between fixing screw and The capillary lays in the grove and should be tied around the inlet fitting.. the body (in the grove) 5 times. Insert the fixing screw, so that the capillary cannot leave Carefully insert the I.D.
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Maintenance Fix the heat exchanger to the clamp unit and the flow cell Fix the inlet capillary to the flow cell body handtight first. body to the heat exchanger.. Then do a 1/4 turn with a 4-mm wrench. Next steps: Check for a centered holder vs.
Maintenance Replacing Capillaries on a Semi-Micro, Micro and High Pressure Flow Cell When required If the capillary is blocked Tools required Two 1/4 inch wrenches for capillary connections Wrench 4 mm for capillary connections Screwdriver Pozi 1 PT3 Parts required For parts see“Semi-Micro Flow Cell”...
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Maintenance Identify the inlet and outlet capillaries. After replacing the outlet capillary, fix it handtight first. Then do a 1/4 turn with a 4-mm wrench. Inlet capillary Outlet capillary To replace the inlet capillary, use a 4-mm wrench for the Unscrew the cell body from the heat exchanger and the fitting.
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Maintenance Use a small flat screw driver to carefully lift off the I.D. tag. Carefully insert the I.D. tag into the new heat exchanger. Shown is the default orientation. See Note on page 114. Shown is the default orientation. See Note on page 114.
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Maintenance Next steps: Check for a centered holder vs. hole. If required adjust with the holder screws. Reconnect the capillaries, see “Exchanging a Flow Cell” on page 103. Perform a leak test. Insert the flow cell. Replace the front cover. Perform a “Wavelength Verification and Recalibration”...
Maintenance Nano Flow Cell - Replacing or Cleaning When required If parts are contaminated or leaky. Tools required Screwdriver POZI 1 PT3 Two 1/4 inch wrenches for capillary connections Parts required For parts identification refer to “Nano Flow Cells” on page 158 (80 nl and 500 nl).
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Maintenance 1 Disconnect the capillaries from the capillary holder and 2 Unscrew the cell body from the holder. remove the flow cell. 3 Unscrew the capillaries from the flow cell. DO NOT use the 4 Using for example a toothpick, press on the plastic part adapter at this time! and slide the quartz body out of the cell housing.
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Maintenance 5 The quartz body and the cell seal assembly can be 6 This figure shows the correct holding of the quartz body separated for cleaning purpose. and the cell seal assembly. 7 Replace the cell seal assembly onto the quartz body. 8 Slide the quartz body completely into the cell body to the Always use a new seal assembly to exclude damage front stop (use for example a toothpick).
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Maintenance 9 Insert the flow cell capillaries and tighten them 10 Reassemble the flow cell body to the holder. fingertight. Use the wrench and torque adapter as described on page 127 and tighten the fittings alternately. 11 Re-install the flow cell and connect the capillaries to the Next Steps: union holder.
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Maintenance With the instrument accessory kit comes a 4-mm wrench and with the Sealing Kit a special N O T E adapter. Both together work as a torque wrench with pre-defined torque (maximum allowed torque for the cell fittings is 0.7 Nm). It can be used to tight the capillary fittings at the flow cell body.
Maintenance Cleaning or Exchanging the Holmium Oxide Filter When required If holmium oxide filter is contaminated Tools required Screwdriver POZI 1 PT3 Screwdriver flat blade Two 1/4 inch wrenches for capillary connections A pair of tweezers Parts required Holmium oxide filter 79880-22711 Preparations Turn the lamp(s) off.
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Maintenance 1 Unscrew the six screws and remove the flow cell cover. 2 If not already in this position, move the filter up. 3 While releasing the holder with a screwdriver, carefully Note: remove the holmium oxide filter using a pair of tweezers Do not scratch the holmium oxide filter.
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Maintenance 4 While releasing the holder with a screw driver, carefully 5 Replace the flow cell cover and fix the six screws. insert the holmium oxide filter. Next steps: 6 Perform a “Wavelength Verification and Recalibration” on page 138 to check the proper function of the holmium oxide filter. 7 Insert the flow cell, see “Exchanging a Flow Cell”...
Maintenance Correcting Leaks When required If a leakage has occurred in the flow cell area or at the heat exchanger or at the capillary connections Tools required Tissue Two 1/4 inch wrenches for capillary connections Parts required None Preparations Remove the front cover. 1 Use tissue to dry the leak sensor area and the leak pan.
Maintenance Replacing Leak Handling System Parts When required If the parts are corroded or broken Tools required None Parts required Leak funnel 5061-3388 Leak funnel holder 5041-8389 Leak tubing (120 mm) 0890-1711 Preparations Remove the front cover. 1 Pull the leak funnel out of the leak funnel holder. 2 Pull out the leak funnel with the tubing.
Maintenance Replacing the Interface Board When required For all repairs inside the detector or for installation of the board Part required Interface board (BCD) G1351-68701 with external contacts and BCD outputs, LAN Communication Interface board G1369A or G1369-60001. Tools required None Preparations •...
2.10 or above and the documentation from the Agilent web http://www.chem.agilent.com/scripts/cag_firmware.asp. 2 Load the firmware into the detector as described in the documentation. The G1315B DAD and the G1365B MWD require firmware revision A.04.x or above (main N O T E and resident).
Maintenance Tests & Calibrations The following tests are required after maintenance of lamps and flow cells: “Intensity Test” on page 136. • “Wavelength Verification and Recalibration” on page 138. • • “Holmium Oxide Test” on page 139. • “Cell Test (ChemStation only)” on page 141.
Maintenance Intensity Test The test is for the standard flow cells (10 mm and 6 mm pathlength) only. The nano-flow N O T E cells (80 nl and 500 nl) cannot be run with this test due to its low volume. The intensity test measures the intensity of the deuterium and tungsten lamps over the full wavelength range (190 –...
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Maintenance Suggested Actions ✔ Ensure the flow cell is filled with water, and free from air bubbles. ✔ Run the cell test (see “Cell Test (ChemStation only)” on page 141). If the test fails, exchange the flow cell windows. ✔ Clean optical components with alcohol and lint-free cloth.
Maintenance Wavelength Verification and Recalibration The detector uses the alpha (656.1 nm) and beta (486 nm) emission lines of the deuterium lamp for wavelength calibration. The sharp emission lines enable more accurate calibration than is possible with holmium oxide. When verificaation is started, the 1-nm slit is moved into the light path automatically, and the gain is set to zero.
Maintenance Holmium Oxide Test The holmium oxide test uses three characteristic absorbance maxima of the built-in holmium oxide filter to verify wavelength accuracy (see also “Wavelength Verification and Recalibration” on page 138). When the test is started, the 1-nm slit is moved into the light path automatically. To eliminate effects due to absorbing solvents, the test should be done with water in the flow cell.
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Maintenance Suggested Actions ✔ Ensure the flow cell is filled with water. ✔ Recalibrate (see “Wavelength Verification and Recalibration” on page 138) and repeat the test. ✔ Run the cell test (see “Cell Test (ChemStation only)” on page 141). If the test fails, exchange the flow cell windows.
Maintenance Cell Test (ChemStation only) The cell test measures the intensity of the deuterium and tungsten lamps over the full wavelength range (190 – 950 nm), once with the flow cell installed, and once with the flow cell removed. The resulting intensity ratio is a measure of the amount of light absorbed by the flow cell.
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Maintenance Test Failed (low ratio value) Probable Causes • Absorbing solvent or air bubble in flow cell. • Dirty or contaminated flow cell. Suggested Actions ✔ Ensure the flow cell is filled with water, and free from air bubbles. Exchange the flow cell windows. 1200 Series DAD and MWD User Manual...
Overview of Maintenance Parts Standard Flow Cell Semi-Micro Flow Cell Micro Flow Cell High Pressure Flow Cell Prep Flow Cell - SST Prep Flow Cell - Quartz Nano Flow Cells Accessory Kit This chapter provides information on parts for maintenance. Agilent Technologies...
Parts and Materials for Maintenance Overview of Maintenance Parts 1200 Series DAD and MWD User Manual...
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Parts and Materials for Maintenance Table 16 Maintenance Parts Item Description Part Number Front cover 5065-9982 Control Module G1323B or G1323-67001 Instant Pilot G4208A G4208-67001 Flow Cells with ID tag. For details see “Standard Flow Cell” on page 146, “Semi-Micro Flow Cell”...
Parts and Materials for Maintenance Standard Flow Cell Standard Flow Cell Parts Table 17 Item Description Part Number Standard flow cell assembly, 10 mm, 13 µl, G1315-60022 maximum pressure 120 bar (12 MPa), with I.D. tag Window screw 79883-22402 Spring washers, pack of 10 5062-8553 Compression washer 79883-28801...
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Parts and Materials for Maintenance NOTE Gaskets # 6 and #7 have different hole diameters. Figure 46 Standard Flow Cell Parts 1 - window screw 2 - spring washers 3 - compression washer 4 - window holder 5 - quartz window 6 - Gasket Figure 47 Orientation of Spring Washers.
Parts and Materials for Maintenance Semi-Micro Flow Cell Semi-Micro Flow Cell Parts Table 18 Item Description Part Number Semi-micro flow cell assembly, 6 mm, 5 µl, G1315-60025 maximum pressure 120 bar (12 MPa), with I.D. tag Window screw 79883-22402 Spring washers, pack of 10 5062-8553 Compression washer 79883-28801...
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Parts and Materials for Maintenance NOTE Gaskets # 6 and #7 have different hole diameters. Figure 48 Semi-Micro Flow Cell Parts 1 - window screw 2 - spring washers 3 - compression washer 4 - window holder 5 - quartz window 6 - Gasket Figure 49 Orientation of Spring Washers.
Parts and Materials for Maintenance Micro Flow Cell Micro Flow Cell Parts Table 19 Item Description Part Number Micro flow cell assembly, 3 mm, 2 µl, G1315-60024 maximum pressure 120 bar (12 MPa) Window screw 79883-22402 Spring washers, pack of 10 5062-8553 Compression washer 79883-28801...
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Parts and Materials for Maintenance NOTE Gaskets # 6 and #7 have different hole diameters. Figure 50 Micro Flow Cell Parts 1 - window screw 2 - spring washers 3 - compression washer 4 - window holder 5 - quartz window 6 - Gasket Figure 51 Orientation of Spring Washers.
Parts and Materials for Maintenance High Pressure Flow Cell High Pressure Flow Cell Parts Table 20 Item Description Part Number High pressure flow cell assembly, 6 mm, 1.7 µl, G1315-60015 maximum pressure 400 bar (40 MPa) Window assembly, comprises items 2, 3, 4, 5 and 6 Seal ring 79883-27101 Quartz window...
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Parts and Materials for Maintenance Figure 52 High Pressure Flow Cell Parts 1200 Series DAD and MWD User Manual...
Parts and Materials for Maintenance Prep Flow Cell - SST For more details on the Preparative Flow Cells refer to the technical note that comes with N O T E the flow cells. Table 21 Prep Flow Cell - SST Parts Item Description Part Number...
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Parts and Materials for Maintenance Table 21 Prep Flow Cell - SST Parts, continued Item Description Part Number Handle for clamp unit G1315-84901 Clamp unit G1315-84902 Screw M 2.5, 4 mm lg for cell body/clamp 0515-1056 9 - inlet NOTE 9 - outlet Gaskets # 6 and #7 have different hole diameters.
Parts and Materials for Maintenance Prep Flow Cell - Quartz For more details on the Preparative Flow Cells refer to the technical note that comes with N O T E the flow cells. Table 22 Prep Flow Cell - Quartz Parts Item Description Part Number...
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Parts and Materials for Maintenance 1 - outlet 1 - inlet Figure 55 Prep Flow Cell - Quartz Parts 1200 Series DAD and MWD User Manual...
Parts and Materials for Maintenance Nano Flow Cells The following kits are available: Table 23 Nano-flow cell kits Description Part number 500 nl Flow Cell Kit G1315-68724 includes Flow cell assembly (10 mm, 500 nl, 5 MPa) completely assembled (includes items 1, 2, 3, 4, 10, 11, 12, 13, 14, 15, and 16) 80 nl Flow Cell Kit G1315-68716 includes Flow cell assembly (10 mm, 500 nl, 5 MPa) completely...
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Parts and Materials for Maintenance Table 24 lists the generic parts for both nano-flow cells: Table 24 Generic Parts Item Description Part Number Fitting Screw (for 4 mm wrench), QTY=2 (reorder 10/pk) 5063-6593 Cell ferrules are factory installed PEEK fitting 1/32" (not attached to capillaries), (reorder 10/pk) 5065-4422 Litetouch ferrules LT-100, (1/32"...
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Parts and Materials for Maintenance Table 25 lists the specific parts for the 500 nl flow cell. Table 25 Specific 500 nl Flow Cell Parts Item Description Part Number 500 nl Flow Cell Kit G1315-68724 PEEK coated fused silica capillary Inlet (100 µm) G1315-87333 pre-mounted to cell, includes Inlet capillary, 300 mm long, 100 µm i.d.
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Parts and Materials for Maintenance Table 26 lists the specific parts for the 80 nl flow cell. Table 26 Specific 80 nl Flow Cell Parts Item Description Part Number 80 nl Flow Cell Kit G1315-68716 PEEK coated fused silica capillary Inlet (50 µm) G1315-87323 pre-mounted to cell, includes Inlet capillary, 400 mm long, 50 µm i.d.
Parts and Materials for Maintenance Accessory Kit This kit contains some accessories and tools needed for the installation and repair of the detector. Table 27 Accessory Kit Parts Item Description Part Number Accessory kit G1315-68705 Corrugated tubing (to waste), re-order 5 m 5062-2463 Teflon Tubing flexible i.d.
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Parts and Materials for Maintenance Figure 57 Waste Tubing Parts This end is pre-installed Figure 58 Inlet Capillary (Column-Detector) Parts 1200 Series DAD and MWD User Manual...
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Parts and Materials for Maintenance 1200 Series DAD and MWD User Manual...
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General Safety Information Lithium Batteries Information The Waste Electrical and Electronic Equipment (WEEE) Directive (2002/96/EC) Radio Interference Sound Emission UV-Radiation Solvent Information Declaration of Conformity for HOX2 Filter Agilent Technologies on Internet This chapter provides safetey and other general information. Agilent Technologies...
Appendix General Safety Information The following general safety precautions must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Aligent Technologies assumes no liability for the customer’s failure to comply with these requirements.
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Appendix The operator of this instrument is advised that if the equipment is used in a manner not C A U T I O N specified in this manual, the protection provided by the equipment may be impaired. Some adjustments described in the manual, are made with power supplied to the instrument, and protective covers removed.
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Appendix Safety Symbols Table 28 shows safety symbols used on the instrument and in the manuals. Table 28 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect the apparatus against damage.
Appendix Lithium Batteries Information Danger of explosion if battery is incorrectly replaced. Replace only with the same or WA R N I N G equivalent type recommended by the equipment manufacturer. Lithium batteries may not be disposed-off into the domestic waste. Transportation of discharged Lithium batteries through carriers regulated by IATA/ICAO, ADR, RID, IMDG is not allowed.
Appendix The Waste Electrical and Electronic Equipment (WEEE) Directive (2002/96/EC) Abstract The Waste Electrical and Electronic Equipment (WEEE) Directive (2002/96/EC), adopted by EU Commission on 13 February 2003, is introducing producer responsibility on all Electric and Electronic appliances from 13 August 2005. This product complies with the WEEE Directive (2002/96/EC) N O T E marking requirements.
Appendix Radio Interference Never use cables other than the ones supplied by Aligent 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.
Appendix Sound Emission Manufacturer’s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991. This product has a sound pressure emission (at the operator position) < 70 dB. • Sound Pressure Lp < 70 dB (A) •...
Appendix UV-Radiation This information is only valid for UV-lamps without cover (e.g. 2140-0590 and 2140-0813 N O T E Emissions of ultraviolet radiation (200-315 nm) from this product is limited such that radiant exposure incident upon the unprotected skin or eye of operator or service personnel is limited to the following TLVs (Threshold Limit Values) according to the American Conference of Governmental Industrial Hygienists:...
Appendix Solvent Information Observe the following recommendations on the use of solvents. Flow Cell Avoid the use of alkaline solutions (pH > 9.5) which can attack quartz and thus impair the optical properties of the flow cell. Prevent any crystallization of buffer solutions. This will lead into a blockage/damage of the flow cell.
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Appendix • Chromatographic grade ethers, which can contain peroxides (for example, THF, dioxane, di-isopropylether) such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides. • Solutions of organic acids (acetic acid, formic acid, and so on) in organic solvents.
Appendix Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at: http://www.agilent.com Select “Products” - “Chemical Analysis” It will provide also the latest firmware of the Agilent 1200 Series modules for download.
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Appendix 1200 Series DAD and MWD User Manual...
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Index installation accessory kit, accessory kit, 31, early maintenance feedback (EMF), bench space, accuracy of wavelength, electrical connections delivery checklist, achromat (source lens), description of, environment, Agilent on internet, location of connectors, flow connections, algea information, EMF (early maintenance feedback), of flow cell and capillaries, alpha and beta line, entrance slit,...
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Index settings, spectrograph, 13, operation temperature, rear view of module, diodes per nm, optical system recalibration of wavelength, stack configuration, 32, diagram, repairs front view, overview, cleaning the instrument, rear view, optimization correction leaks, standard flow cell choosing a flow cell, definition of, dimensions, detector performance,...