Agilent Technologies 1260 Infinity G1315C, User Manual

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Agilent Technologies 1260 Infinity G1315C User Manual Download Page 63

Agilent 1260 Infinity DAD and MWD User Manual

63

Using the Detector

4

Setting up an Analysis

Setting up an Analysis

This chapter may be used to

•

Prepare the system,

•

Get to know the set up of an HPLC analysis and

•

Use it as an instrument check to demonstrate that all modules of the system
are correctly installed and connected. It is not a test of the instrument
performance.

•

Learn about special settings

Before Using the System

Solvent Information

Observe recommendations on the use of solvents in chapter “Solvents”.

Priming and Purging the System

When the solvents have been exchanged or the pumping system has been
turned off for a certain time (for example, overnight) oxygen will re-diffuse
into the solvent channel between the solvent reservoir, vacuum degasser
(when available in the system) and the pump. Volatile ingredients will
evaporate to some extend. Therefore priming of the pumping system is
required before starting an application.

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Summary of Contents for 1260 Infinity G1315C

Page 1: ...Agilent Technologies Agilent 1260 Infinity Diode Array and Multiple Wavelength Detector User Manual ...

Page 2: ...ribed in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or sub contract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 ...

Page 3: ... provides information on environmental requirements physical and performance specifications 3 Installing the Module This chapter gives information about the preferred stack setup for your system and the installation of your module 4 Using the Detector This chapter provides information on how to set up the detector for an analysis and explains the basic settings 5 How to optimize the Detector This ...

Page 4: ...pter describes the maintenance of the detector 10 Parts for Maintenance This chapter provides information on parts for maintenance 11 Identifying Cables This chapter provides information on cables used with the Agilent 1200 Infinity Series modules 12 Hardware Information This chapter describes the detector in more detail on hardware and electronics 13 LAN Configuration This chapter provides inform...

Page 5: ...izing the Stack Configuration 40 Installation Information on Leak and Waste Handling 44 Installing the Detector 48 Flow Connections to the Detector 51 Installing Capillaries 54 Setting up the LAN access 60 4 Using the Detector 61 Leak and Waste Handling 62 Setting up an Analysis 63 Special Settings of the Detector 78 Special Setups with Multiple DAD MWDs 92 Solvent Information 93 5 How to optimize...

Page 6: ... Chromatogram 158 Wavelength Verification and Calibration 160 9 Maintenance 163 Introduction to Maintenance 164 Cautions and Warnings 165 Overview of Maintenance 167 Cleaning the Module 168 Exchanging a Lamp 169 Exchanging a Flow Cell 172 Maintenance of Standard Semi Micro or Micro Flow Cell 176 Maintenance of High Pressure Flow Cell 180 Replacing Capillaries on a Standard Flow Cell 182 Replacing ...

Page 7: ...te Cables 234 BCD Cables 237 CAN LAN Cables 239 Agilent 1200 module to PC 240 12 Hardware Information 241 Firmware Description 242 Electrical Connections 245 Interfaces 247 Setting the 8 bit Configuration Switch 254 Instrument Layout 258 Early Maintenance Feedback EMF 259 13 LAN Configuration 261 What you have to do first 262 TCP IP parameter configuration 263 Configuration Switch 264 Initializati...

Page 8: ...e Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 295 Radio Interference 296 Sound Emission 297 UV Radiation 298 Solvent Information 299 Declaration of Conformity for HOX2 Filter 301 Installation of Stainless Steel Cladded PEEK Capillaries 302 Agilent Technologies on Internet 308 ...

Page 9: ...Agilent Technologies 1 Introduction Introduction to the Detector 10 Optical System 11 System Overview 14 Leak and Waste Handling 14 Bio inert Materials 16 This chapter gives an introduction to the detector instrument overview and internal connectors ...

Page 10: ...mps for highest intensity and lowest detection limit over a wavelength range of 190 950 nm no loss in sensitivity for up to eight wavelengths simultaneous programmable slit from 1 16 nm for complete optimization of sensitivity linearity and spectral resolution optional flow cell cartridges with RFID tag standard 10 mm13 μL semi micro 6 mm5 μL micro 3 mm2 μL 80 nL 500 nL 10 mm high pressure 10 mm1 ...

Page 11: ... lamp by means of a special rear access lamp design which allows both light sources to be optically combined and share a common axis to the source lens The achromat source lens forms a single focused beam of light through the flow cell Each cell room and lamp are separated by a quartz window which can be cleaned or replaced In the spectrograph light is being dispersed onto the diode array by a hol...

Page 12: ...rograph material is ceramic to reduce thermal effects to a minimum The spectrograph consists of the spectrograph lens the variable entrance slit the grating and the photodiode array with front end electronics The spectrograph lens refocuses the light beam after it has passed through the flow cell The sampling interval of the diode array is 1 nm over the wavelength range 190 950 nm Depending on the...

Page 13: ...ed by using a concave holographic grating The grating separates the light beam into all its component wavelengths and reflects the light onto the photodiode array 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 ...

Page 14: ...iew Leak and Waste Handling The 1200 Infinity Series has been designed for safe leak and waste handling It is important that all security concepts are understood and instructions are carefully followed Figure 2 Leak and waste handling concept overview typical stack configuration as an example ...

Page 15: ...on internal parts e g the detector s flow cell The leak sensor in the leak pan stops the running system as soon as the leak detection level is reached The leak pan s outlet port 3 A guides excessive overfill from one module to the next as the solvent flows into the next module s leak funnel 3 B and the connected corrugated waste tube 3 C The corrugated waste tube guides the solvent to the next low...

Page 16: ...ary Pump G5611A Titanium gold platinum iridium ceramic ruby PTFE PEEK Agilent 1260 Infinity Bio inert High Performance Autosampler G5667A Upstream of sample introduction Titanium gold PTFE PEEK ceramic Downstream of sample introduction PEEK ceramic Agilent 1260 Infinity Bio inert Manual Injector G5628A PEEK ceramic Agilent 1260 Infinity Bio inert Analytical Fraction Collector G5664A PEEK ceramic P...

Page 17: ...eam of sample introduction Agilent uses stainless steel cladded PEEK capillaries which keep the flow path free of steel and provide pressure stability to more than 600 bar Table 1 Bio inert materials used in Agilent 1260 Infinity Systems Module Materials NOTE To ensure optimum bio compatibility of your Agilent 1260 Infinity Bio inert LC system do not include non inert standard modules or parts to ...

Page 18: ...18 Agilent 1260 Infinity DAD and MWD User Manual 1 Introduction Bio inert Materials ...

Page 19: ...es 2 Site Requirements and Specifications Site Requirements 20 Physical Specifications 23 Performance Specifications 24 Specifications 24 Specification Conditions 36 This chapter provides information on environmental requirements physical and performance specifications ...

Page 20: ... result if the devices are connected to a line voltage higher than specified Connect your instrument to the specified line voltage only WARNING The module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g electrical shock when the cover is opened and the module is connected to power Always unplug the power c...

Page 21: ...hock or short circuit Never operate your instrumentation from a power outlet that has no ground connection Never use a power cord other than the Agilent Technologies power cord designed for your region WARNING Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury Never use cables other than the ones supplied by...

Page 22: ...r one hour period Our published drift specification refer also to Performance Specifications G1315C on page 24 is based on these conditions Larger ambient temperature changes will result in larger drift Better drift performance depends on better control of the temperature fluctuations To realize the highest performance minimize the frequency and the amplitude of the temperature changes to below 1 ...

Page 23: ... V 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 160 VA 160 W 546 BTU Maximum Ambient operating temperature 0 55 C 32 131 F Ambient non operating temperature 40 70 C 40 158 F Humidity 95 r h at 40 C 104 F Non condensing Operating altitude Up to 3000 m 9842 ft Non operating altitude Up to 4600 m 15092 ft For storing the module Safety standards IEC EN CSA UL Installation ...

Page 24: ...ith RFID tag that holds lamp typical information Data rate up to 80 Hz Wavelength range 190 950 nm Short term noise ASTM Single and Multi Wavelength 0 7 10 5 AU at 254 and 750 nm see Specification Conditions below Drift 0 9 10 3 AU h at 254 nm see Specification Conditions below Linear absorbance range 2 AU 5 at 265 nm see Specification Conditions below Wavelength accuracy 1 nm Self calibration wit...

Page 25: ...d 50 bar 725 psi pressure maximum High pressure 1 7 µL volume 6 mm cell path length and 400 bar 5800 psi pressure maximum Prep SST 3 mm cell path length and 120 bar 1740 psi pressure maximum Prep Quartz 0 3 mm cell path length and 20 bar 290 psi pressure maximum Prep Quartz 0 06 mm cell path length and 20 bar 290 psi pressure maximum All flow cells are equipped with RFID tags that hold cell typica...

Page 26: ...e Extensive diagnostics error detection and display through control module and ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features RFID for electronics records of flow cell and UV lamp conditions path length volume product number serial number test passed usage Early maintenance feedback EMF for contin...

Page 27: ...ds lamp typical information Data rate up to 20 Hz Wavelength range 190 950 nm Short term noise ASTM Single and Multi Wavelength 0 7 10 5 AU at 254 and 750 nm see Specification Conditions below Drift 0 9 10 3 AU h at 254 nm see Specification Conditions below Linear absorbance range 2 AU 5 at 265 nm see Specification Conditions below Wavelength accuracy 1 nm Self calibration with deuterium lines ver...

Page 28: ...400 bar 5800 psi pressure maximum Prep SST 3 mm cell path length and 120 bar 1740 psi pressure maximum Prep Quartz 0 3 mm cell path length and 20 bar 290 psi pressure maximum Prep Quartz 0 06 mm cell path length and 20 bar 290 psi pressure maximum All flow cells are equipped with RFID tags that hold cell typical information pH range 1 0 9 5 12 5 solvent dependent with bio inert version Time progra...

Page 29: ...ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features RFID for electronics records of flow cell and UV lamp conditions path length volume product number serial number test passed usage Early maintenance feedback EMF for continuous tracking of instrument usage in terms of lamp burn time with user setable ...

Page 30: ...ds lamp typical information Data rate up to 80 Hz Wavelength range 190 950 nm Short term noise ASTM Single and Multi Wavelength 0 7 10 5 AU at 254 and 750 nm see Specification Conditions below Drift 0 9 10 3 AU h at 254 nm see Specification Conditions below Linear absorbance range 2 AU 5 at 265 nm see Specification Conditions below Wavelength accuracy 1 nm Self calibration with deuterium lines ver...

Page 31: ...ressure maximum Nano 80 nL volume 6 mm cell path length and 50 bar 725 psi pressure maximum High pressure 1 7 µL volume 6 mm cell path length and 400 bar 5800 psi pressure maximum Prep SST 3 mm cell path length and 120 bar 1740 psi pressure maximum Prep Quartz 0 3 mm cell path length and 20 bar 290 psi pressure maximum Prep Quartz 0 06 mm cell path length and 20 bar 290 psi pressure maximum All fl...

Page 32: ...e Extensive diagnostics error detection and display through control module and ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features RFID for electronics records of flow cell and UV lamp conditions path length volume product number serial number test passed usage Early maintenance feedback EMF for contin...

Page 33: ...ds lamp typical information Data rate up to 20 Hz Wavelength range 190 950 nm Short term noise ASTM Single and Multi Wavelength 0 7 10 5 AU at 254 and 750 nm see Specification Conditions below Drift 0 9 10 3 AU h at 254 nm see Specification Conditions below Linear absorbance range 2 AU 5 at 265 nm see Specification Conditions below Wavelength accuracy 1 nm Self calibration with deuterium lines ver...

Page 34: ...ressure maximum Nano 80 nL volume 6 mm cell path length and 50 bar 725 psi pressure maximum High pressure 1 7 µL volume 6 mm cell path length and 400 bar 5800 psi pressure maximum Prep SST 3 mm cell path length and 120 bar 1740 psi pressure maximum Prep Quartz 0 3 mm cell path length and 20 bar 290 psi pressure maximum Prep Quartz 0 06 mm cell path length and 20 bar 290 psi pressure maximum All fl...

Page 35: ...aintenance Extensive diagnostics error detection and display through control module and ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features RFID for electronics records of flow cell and UV lamp conditions path length volume product number serial number test passed usage Early maintenance feedback EMF f...

Page 36: ...nt temperature changes will result in larger drift Better drift performance depends on better control of the temperature fluctuations To realize the highest performance minimize the frequency and the amplitude of the temperature changes to below 1 C hour 1 8 F hour Turbulences around one minute or less can be ignored Performance tests should be done with a completely warmed up optical unit two hou...

Page 37: ...st 39 Optimizing the Stack Configuration 40 Two Stack Configuration 42 Installation Information on Leak and Waste Handling 44 Installing the Detector 48 Flow Connections to the Detector 51 Installing Capillaries 54 Setting up the LAN access 60 This chapter gives information about the preferred stack setup for your system and the installation of your module ...

Page 38: ... Inform your service representative that the instrument may have been damaged during shipment CAUTION Defective on arrival problems If there are signs of damage please do not attempt to install the module Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged Notify your Agilent sales and service office about the damage An Agilent service representative wil...

Page 39: ... below Please report missing or damaged parts to your local Agilent Technologies sales and service office Table 7 Detector Checklist Description Quantity Detector 1 CompactFlash Card 1 installed G1315C G1365C only Power cable 1 Cross over network cable 1 Twisted pair network cable 1 Flow cell As ordered User Manual on Documentation CD part of the shipment not module specific 1 per order Accessory ...

Page 40: ...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 Figure 3 Recommended Stack Configuration for 1260 Infinity Front View HWHFWRU 9DFXXP GHJDVVHU 3XPS XWRVDPSOHU ROXPQ FRPSDUWPHQW 6ROYHQW FDELQHW QVWDQW 3LORW ...

Page 41: ...he Module 3 Optimizing the Stack Configuration Figure 4 Recommended Stack Configuration for 1260 Infinity Rear View SRZHU 1 XV FDEOH WR 1 XV FDEOH QDORJ GHWHFWRU VLJQDO RU RXWSXWV SHU GHWHFWRU 5HPRWH FDEOH 1 WR KHP6WDWLRQ ORFDWLRQ GHSHQGV RQ GHWHFWRU QVWDQW 3LORW ...

Page 42: ...wo stacks Some users prefer the lower height of this arrangement even without the autosampler thermostat A slightly longer capillary is required between the pump and autosampler See Figure 5 on page 42 and Figure 6 on page 43 Figure 5 Recommended Two Stack Configuration for 1260 Infinity Front View QVWDQW 3LORW HWHFWRU ROXPQ FRPSDUWPHQW 6ROYHQW FDELQHW HJDVVHU RSWLRQDO 3XPS 7KHUPRVWDW IRU WKH 6 UD...

Page 43: ... 43 Installing the Module 3 Optimizing the Stack Configuration Figure 6 Recommended Two Stack Configuration for 1260 Infinity Rear View 1 WR FRQWURO VRIWZDUH 1 XV FDEOH WR QVWDQW 3LORW 1 XV FDEOH 5HPRWH FDEOH 3RZHU XWRVDPSOHU UDFWLRQ ROOHFWRU DEOH ...

Page 44: ...s safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice The volume of substances should be reduced to the minimum required for the analysis Never exceed the maximal permissible volume of solvents 6 L in the solvent cabinet Do not use bottles that exceed the maximum permissible volume as specified...

Page 45: ...ing Figure 7 Leak and waste handling overview typical stack configuration as an example 1 Solvent cabinet 2 Leak pan 3 Leak pan s outlet port A leak funnel B and corrugated waste tube C 4 Waste tube of the sampler s needle wash 5 Condense drain outlet of the autosampler cooler 6 Waste tube of the purge valve 7 Waste tube ...

Page 46: ...elow 3 Connect capillaries and tubes to the modules see section Flow Connections to the module below or the relevant system manual WARNING Toxic flammable and hazardous solvents samples and reagents Keep solvent path free from blockages Keep the flow path closed in case the pump in the system is equipped with a passive inlet valve solvent may leak out due to hydrostatic pressure even if your instr...

Page 47: ...Agilent 1260 Infinity DAD and MWD User Manual 47 Installing the Module 3 Installation Information on Leak and Waste Handling Figure 8 Warning label illustration for correct waste tubing ...

Page 48: ...ized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened and the module is connected to power Make sure that it is always possible to access the power plug Remove the power cable from the instrument before opening the cover Do not connect the power cable to the Instrument while the covers are re...

Page 49: ... power switch at the front of the module is OFF 4 Connect the power cable to the power connector at the rear of the module Figure 9 Rear View of Detector 5 Connect the CAN cable to other Agilent 1200 Series modules 6 Connect the LAN cable e g from a Agilent ChemStation as controller to the detector s LAN connector 7 Connect the analog cable s optional 8 Connect the APG remote cable optional for no...

Page 50: ...Front View of Detector 6WDWXV LQGLFDWRU JUHHQ HOORZ UHG LQH SRZHU VZLWFK ZLWK JUHHQ OLJKW NOTE The module is turned on when the line power switch is pressed and the green indicator lamp is illuminated The module is turned off when the line power switch is protruding and the green light is off NOTE The module was shipped with default configuration settings To change these settings see Configuration...

Page 51: ...thing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice The volume of substances should be reduced to the minimum required for the analysis Do not operate the instrument in an explosive atmosphere NOTE The flow cell is shipped with a filling of isopropanol also recommended when the instrument and or flow cell is shipped to anothe...

Page 52: ...ed to the bottom or to the top depending on the routing of the capillaries to the column For details see Replacing Capillaries on a Standard Flow Cell on page 182 1 Press the release buttons and remove the front cover to gain access to the flow cell area 2 Press the release button and open the flow cell door 3 Insert the flow cell 4 Connect the flow cell capillaries to the capillary holder top is ...

Page 53: ...rom the accessory kit behind the capillary holder and connect the top end to the other module s waste outlet 6 Connect the capillary from the column to the capillary holder top Connect the PTFE waste tubing to the flow cell outlet fitting bottom and the corrugated waste tubing to the leak outlet 7 Remove the flow cell and establish a flow and observe for leaks 8 Insert the flow cell close the cove...

Page 54: ...e below illustrates the differences between new and previous capillaries Figure 11 New bio inert capillary and UHP FF fitting with nose Figure 12 Previous bio inert capillary and fitting PP ILWWLQJ LQFK ILWWLQJ NOTE For handling instructions of capillaries and fittings used in modules before delivery of the new UHP FF fittings introduced in May 2013 refer to Installation of Stainless Steel Cladded...

Page 55: ...ling UHP FF Fittings 1 Slide the fitting on the capillary Let the capillary jut out 5 mm Tools required p n Description 5043 0915 Fitting mounting tool for bio inert capillaries Parts required p n Description Capillaries and Fittings For details refer to the part section of the manual PP DSLOODU LWWLQJ ...

Page 56: ...finity DAD and MWD User Manual 3 Installing the Module Installing Capillaries 2 Insert the fitting to the receiving port and push the capillary to the bottom of the port 3 Finger tighten the nut into the port until snug ...

Page 57: ...nual 57 Installing the Module 3 Installing Capillaries 4 Use Fitting mounting tool 5043 0915 or a 5 mm hex wrench for fixing the fitting maximum torque 0 8 Nm CAUTION Potential damage of capillaries Do not remove fittings from used capillaries ...

Page 58: ...ries Bio inert capillaries are using a PEEK front end which may expand under pressure especially when being in contact with some organic solvents If a fitting is moved across an expanded PEEK end there is a risk of damaging the capillary by ripping off its end Before re installing such capillaries push the ferrule towards the rear site for a small distance Figure 13 Capillary fitting 6WHS 5HDU URQ...

Page 59: ...pillaries need to be installed in the correct sequence Otherwise an inset of the union may be damaged and the connection may not be tight CAUTION Potential leak or damage of the Bio inert ZDV Union To avoid leaks or a damage to the Bio inert ZDV union follow the procedure below in the prescribed sequence 1 Install the capillary at the end marked with a ring indentation 2 Install the second capilla...

Page 60: ...60 Agilent 1260 Infinity DAD and MWD User Manual 3 Installing the Module Setting up the LAN access Setting up the LAN access Please follow the instructions in LAN Configuration on page 261 ...

Page 61: ... Run Recovery Settings 81 Automated Run Recovery in case of temporary communication failures 82 Manual Run Recovery in case of permanent communication failures 84 Analog Output Settings 85 Spectrum Settings DAD only 86 Peakwidth Settings 88 Slit Settings 90 Margin for Negative Absorbance Settings 91 Optimizing the Detector 91 Special Setups with Multiple DAD MWDs 92 Two detectors of same type e g ...

Page 62: ...um required for the analysis Do not operate the instrument in an explosive atmosphere Never exceed the maximal permissible volume of solvents 6 L in the solvent cabinet Do not use bottles that exceed the maximum permissible volume as specified in the usage guideline for the Agilent 1200 Infinity Series Solvent Cabinets Arrange the bottles as specified in the usage guideline for the solvent cabinet...

Page 63: ...mance Learn about special settings Before Using the System Solvent Information Observe recommendations on the use of solvents in chapter Solvents Priming and Purging the System When the solvents have been exchanged or the pumping system has been turned off for a certain time for example overnight oxygen will re diffuse into the solvent channel between the solvent reservoir vacuum degasser when ava...

Page 64: ...both times Isopropanol Isopropanol Best solvent to flush air out of the system Best solvent to flush air out of the system After an installation Ethanol or Methanol Alternative to Isopropanol second choice if no Isopropanol is available Cleaning the system when using buffers After a solvent change Bidistilled water Bidistilled water Best solvent to re dissolve buffer crystals Best solvent to re di...

Page 65: ...ector standard flow cell installed Agilent ChemStation or Instant Pilot G4208 optional for basic operation or with with the appropriate revisions see Performance Specifications on page 24 System should be correctly set up for LAN communication with the Data System Column Zorbax Eclipse XDB C18 150 mm x 4 6 mm 5 µm 993967 906 Standard Agilent isocratic checkout sample 01080 68704 This 0 5 mL ampoul...

Page 66: ... for this analysis is shown in Figure 14 on page 66 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 Figure 14 Typical Chromatogram with UV detector ...

Page 67: ...e Detector 4 Setting up an Analysis Optimization of the System The settings used for this analysis are specific for this purpose For other applications the system can be optimized in various ways Please refer to the section Optimizing the Detector on page 91 ...

Page 68: ...e monitor 2 Turn on the HPLC modules 3 Start the Agilent ChemStation software If the pump autosampler thermostatted column compartment and detector are found the ChemStation screen should look like shown in Figure below The System status is red Not Ready Figure 15 Initial ChemStation screen Method and Run Control 6 VWHP VWDWXV 2Q OLQH SORW ZLQGRZ GHWDLOV ZLQGRZ ...

Page 69: ...is 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 16 Turning on the HPLC Module ...

Page 70: ... Table 11 on page 70 Figure 17 Stabilization of Baseline both lamps turned on at the same time NOTE For reproducible chromatography the detector and lamp should be on for at least one hour Otherwise the detector baseline may still drift depending on the environment See also section Wander Drift Problems Due to Temperature Changes in the Service Manual Table 11 Baseline drift after lamp turn on exa...

Page 71: ...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 DEF_LC M and press OK Alternative double click on the method in the method window The default LC method parameters are transferred into the modules Figure 18 Loading Default LC Method ...

Page 72: ... Using the Detector Setting up an Analysis 9 Click on the module icons see Figure below and open the Setup of these modules Figure on page 73 shows the detector settings do not change the detector parameters at this time Figure 19 Open the module menu ...

Page 73: ...ication the lamps can be selected one or both peak width depends on the peaks in the chromatogram Peakwidth Settings on page 88 autobalance to zero absorbance on the analog output plus offset at begin and or end of run mechanical slit width can be changed for further optimization Slit Settings on page 90 margin for negative absorbance Margin for Negative Absorbance Settings on page 91 Under More a...

Page 74: ...on and select Change to open the Signal Plot information Select the Pump Pressure and the DAD A Signal 254 4 as signals Change the Y range for the DAD to 1 mAU and the offset to 20 and the pressure offset to 50 The X axis range should be 15 minutes Press OK to exit this screen Figure 20 Edit Signal Plot Window ...

Page 75: ...ce signals Pressing Adjust the signals can be reset to the offset value and Balance would do a balance on the detector Figure 21 Online Plot Window 13 If both baselines are stable set the Y range for the detector signal to 100 mAU 3XPS SUHVVXUH VLJQDO DEVRUEDQFH VLJQDO NOTE If you start with a new UV lamp for the first time the lamp may show initial drift for some time burn in effect ...

Page 76: ... menu item RunControl Sample Info and enter information about this application see figure below Press OK to leave this screen Figure 22 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 ...

Page 77: ...a run select the menu item RunControl Run Method 2 This will start the modules and the online plot on the Agilent ChemStation will show the resulting chromatogram Figure 23 Chromatogram with Isocratic Test Sample NOTE Information about using the Data Analysis functions can be obtained from the Using your ChemStation manual supplied with your system ...

Page 78: ...he Agilent ChemStation B 02 01 Control Settings Figure 24 Detector control settings Lamps turn on and off of UV and Vis lamp At Power On automatic lamp on at power on Error Method take error method or current method in case of an error Analog Output Range can be set to either 100 mV or 1 V full scale Analog Output Settings on page 85 Automatic Turn On lamps can be programmed detector must be on fo...

Page 79: ...Cell tag for Agilent flow cells with I D tags If no I D tag cell is used detector icon will become grey cell tag not ready and analysis is disabled Help online help Figure 25Detector configuration settings The detector status shows Cell tag in yellow in case the flow cell with the I D tag is not inserted The detector icon is gray and the system is not ready NOTE If the flow cell temperature is cri...

Page 80: ...nual 4 Using the Detector Special Settings of the Detector Online Spectra DAD only 1 To view the online spectra during the run select Online Spectra Figure 26 Online Spectra Window 2 Change the absorbance and wavelength range according your needs ...

Page 81: ...o loss of data occurs If there is a permanent network failure the Run Recovery dialog box allows you to restore the stored data to the data directory From there you can copy the files to the directory where the files are corrupted or not complete CAUTION For this recovery mode the CompactFlash Card must be in the detector If the LAN communiaction is interruppted no data is stored Have the CompactF...

Page 82: ...Data Analysis Run Rawdata Elapsed run time is running Spectra counter is running Data are stored on PC and on card LAN breaks Run in progress Data Analysis Run Rawdata Error Power Fail Elapsed run time stops Spectra counter stops Data continues to be stored on card LAN recovers Run in progress Data Analysis Run Rawdata Error Power Fail cleared Elapsed run time continues at actual time Data continu...

Page 83: ... Spectra counter continues ChemStation continues to add missing data Run ends Ready Run finished Prerun Ready Table 12 Automated Run Recovery in case of temporary communication failures Situation Reaction On ChemStation NOTE If the detector status window is not opened you will realize only the Power Fail error and the long Run In Progress information until the data is recovered from disk ...

Page 84: ...ery in case of permanent communication failures see Note below Start a recover After a recover 5XQ 5HFRYHU LQ 3URFHVV NOTE When during recovery an error Method Sequence stopped appears the instrument logbook shows an entry No Run data available in device In this case refer to No Run Data Available In Device on page 141 ...

Page 85: ...tputs see Control Settings on page 78 1 To change the offset and the attenuation select Analog Outputs 2 Change the ranges for absorbance and wavelength according your needs 3 Change the values if required Figure 27 Analog Output Settings 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 scale ...

Page 86: ... only 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 13 on page 87 shows the possible parameters 3 Change the Range Step width and Threshold according to your needs Figure 28 Spectra Settings ...

Page 87: ...akwidth parameters set in the integration events Every 2nd spectrum Spectra are taken continuously as for All but only every second spectrum is stored other spectra are discarded This reduces the amount of data storage necessary All Spectra are taken continuously depending on the setting of the Peakwidth Eight spectra are acquired per Peakwidth The acquisition time for one spectrum is slightly les...

Page 88: ...our chromatogram The peak width sets the optimum response time for your detector The peak detector ignores any peaks that are considerably narrower or wider than the peak width setting The response time is the time between 10 and 90 of the output signal in response to an input step function When the All spectrum storage option is selected then spectra are acquired continuously depending on the set...

Page 89: ...me sec Data Rate Hz Detector 0 0025 0 025 80 G1315C G1365C only 0 0025 0 05 80 G1315C G1365C only 0 005 0 1 40 G1315C G1365C only 0 01 0 2 20 G1315C D and G1365C D 0 03 0 5 10 G1315C D and G1365C D 0 05 1 0 5 G1315C D and G1365C D 0 10 2 0 2 5 G1315C D and G1365C D 0 20 4 0 1 25 G1315C D and G1365C D 0 40 8 0 0 62 G1315C D and G1365C D 0 85 16 0 0 31 G1315C D and G1365C D ...

Page 90: ...list 3 Change the Slit width according to your needs The Slit group allows you to select the optical bandwidth of the detector the narrower the slit the smaller the optical bandwidth of the instrument but the lower its sensitivity The smaller the optical bandwidth the higher the spectral resolution To set the slit width display the drop down list and select an appropriate slit width from the list ...

Page 91: ...Additional theoretical information can be found in chapter How to optimize the Detector on page 99 Use this field to modify the detector s signal handling to increase the margin for negative absorbance Use this option if for example your solvent gradient produces a decreasing baseline absorbance and for GPC analyses Limits 100 to 4000 mAU Figure 31 Margin for Negative Absorbance NOTE The higher th...

Page 92: ...ific detector as detector 1 and 2 Two detectors of similar type e g G1315C D and G1315A B If you have similar detectors in the same system the G1315C D will be automatically always detector 2 while the G1315A B is detector 1 independent from its location in the stack This cannot be changed NOTE The G1315C D and G1365C D detectors are based on the same new hardware electronic platform The G1315A B ...

Page 93: ...PLC conditions For any special conditions please consult the material information section or contact Agilent Disclaimer Subsequent data were collected from external resources and are meant as a reference Agilent cannot guarantee the correctness and completeness of such information Data is based on compatibility libraries which are not specific for estimating the long term life time under specific ...

Page 94: ...plers One supplier of polyimide is DuPont which brands polyimide as Vespel which is also used by Agilent Polyimide is stable in a pH range between 1 and 10 and in most organic solvents It is incompatible with concentrated mineral acids e g sulphuric acid glacial acetic acid DMSO and THF It is also degraded by nucleophilic substances like ammonia e g ammonium salts in basic conditions or acetates P...

Page 95: ...cids like nitric acid sulfuric acid and organic solvents especially at higher temperatures replace if your chromatography method allows by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2 CHCl3 O2 2 COCl2 2 HCl This reaction in which stainless steel probably acts as a catalyst occurs...

Page 96: ...roded by strong bases and should not be used above pH 12 at room temperature The corrosion of flow cell windows can negatively affect measurement results For a pH greater than 12 the use of flow cells with sapphire windows is recommended Gold Gold is inert to all common HPLC solvents acids and bases within the specified pH range It can be corroded by complexing cyanides and concentrated acids like...

Page 97: ...ich are used in all Agilent degassers except G1322A are not compatible with fluorinated solvents like Freon Fluorinert or Vertrel They have limited life time in the presence of Hexafluoroisopropanol HFIP To ensure the longest possible life with HFIP it is best to dedicate a particular chamber to this solvent not to switch solvents and not to let dry out the chamber For optimizing the life of the p...

Page 98: ...98 Agilent 1260 Infinity DAD and MWD User Manual 4 Using the Detector Solvent Information ...

Page 99: ...3 Flow Cell Path Length 103 Peak width response time 105 Sample and Reference Wavelength and Bandwidth 107 Slit Width 110 Optimizing Spectral Acquisition DAD only 112 Margin for Negative Absorbance 112 Optimizing Selectivity 113 Quantifying Coeluting Peaks by Peak Suppression 113 Ratio Qualifiers for Selective Detection of Compound Classes 115 This chapter provides information on how to optimize t...

Page 100: ...ity selectivity and linearity spectral sensitivity and resolution DAD only and disk space required for storing data How to Get the Best Detector Performance The information below will guide you on how to get the best detector performance Follow these rules as a start for new applications It gives rules of thumb for optimizing detector parameters NOTE The information in this chapter should be seen ...

Page 101: ...ivity versus disk space Use peak width according Figure 32 on page 102 as starting point Set the peak width close to the width of a narrow peak of interest in your chromatogram 4 Setting wavelength and bandwidth Sample wavelength Never miss a peak by the use of a browser wavelength like 250 nm with 100 nm bandwidth Select specific wavelength with reduced bandwidth if you need selectivity e g 250 1...

Page 102: ...de according to your needs see Table 13 on page 87 Set the spectral wavelength range for colorless samples 190 400 nm is sufficient Set step to 4 nm for normal use set small step and slit width if high resolution of spectra with fine structure is wanted spectral resolution sensitivity and linearity Table 15 Optimization Overview Parameter Impact FP FP PLQ PLQ PLQ PLQ QWHUQDO FROXPQ GLDPHWHU PP PP ...

Page 103: ...cies and d m is the path length of the cell used for the measurement Therefore flow cells with longer path lengths yield higher signals Although noise usually increases little with increasing path length there is a gain in signal to noise ratio For example in Figure 33 on page 104 the noise increased by less than 10 but a 70 increase in signal intensity was achieved by increasing the path length f...

Page 104: ...ils of the flow cells EVRUEDQFH 7LPH PLQ QDO VLV RI SHVWLFLGH VWDQGDUG PP RSWLFDO SDWK OHQJWK PP RSWLFDO SDWK OHQJWK Table 16 Correction factors for flow cells Flow cell Path length actual Correction factor Standard flow cell 10 mm 13 µL 120 bar 12 MPa G1315 60022 9 80 0 07 mm 10 9 8 Semi micro flow cell 6 mm 5 µL 120 bar 12 MPa G1315 60025 5 80 0 07 mm 6 5 8 Micro flow cell 3 mm 2 µL 120 bar 12 M...

Page 105: ...re chromatograms and spectra Figure 34 Influence of Response Time on Signal and Noise Table 17 on page 106 lists the filter choices of the detector To get optimum results set peak width as close as possible to a narrow peak of interest in your chromatogram Response time will the be approximately 1 3 of the peak width resulting in less than 5 peak height reduction and less than 5 additional peak di...

Page 106: ...h minutes Response Time seconds Data Rate Hz Detector 0 0025 0 025 80 G1315C G1365C only 0 0025 0 05 80 G1315C G1365C only 0 005 0 1 40 G1315C G1365C only 0 01 0 2 20 G1315C D and G1365C D 0 03 0 5 10 G1315C D and G1365C D 0 05 1 0 5 G1315C D and G1365C D 0 10 2 0 2 5 G1315C D and G1365C D 0 20 4 0 1 25 G1315C D and G1365C D 0 40 8 0 0 62 G1315C D and G1365C D 0 85 16 0 0 31 G1315C D and G1365C D ...

Page 107: ...mple bandwidth BW and optionally reference wavelength the center of a wavelength band with the width of reference bandwidth 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 avera...

Page 108: ...ng 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 The signal to noise ratio for a 30 nm bandwidth is twice that for a 4 nm bandwidth in our example Figure 36 Influence of Bandwidth on Signal and Noise 5HIHUHQFH EDQGZLGWK QP 5HIHUHQFH ZDYHOHQJWK QLVLF DFLG DYHOHQJWK QP EVRUEDQFH P...

Page 109: ...ve index changes during a gradient An example of the reduction of baseline drifts is shown in Figure 37 on page 109 for PTH amino acids Without a reference wavelength the chromatogram drifts downwards due to refractive index changes induced by the gradient This is almost completely eliminated by using a reference wavelength With this technique PTH amino acids can be quantified in the low picomole ...

Page 110: ...ng demand of different analytical problems A narrow slit provides spectral resolution for analytes with very fine structures in the absorbance spectrum An example of such a spectrum is benzene The five main absorbance bands fingers are only 2 5 nm wide and just 6 nm apart from each other Figure 38 Benzene at 1 4 and 16 nm slit width principle A wide slit uses more of the light shining through the ...

Page 111: ...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 Figure 35 on page 108 In most situations a slit width of 4 nm will give the best results Use a narrow slit 1 or 2 nm if you want to identify compounds with fine spectral structures or if you need to quanti...

Page 112: ...ty checks and library searches Reducing the spectrum storage range saves disk space Step Most substances have broad absorbance bands Display of spectra peak purity and library search works best if a spectrum contains 5 to 10 data points per width of the absorbance bands For anisic acid the example used before a step of 4 nm would be sufficient However a step of 2 nm gives a more optimal display of...

Page 113: ...cedure is called peak suppression or signal subtraction As an example the analysis of hydrochlorothiazide in the presence of caffeine is described If hydrochlorothiazide is analyzed in biological samples there is always a risk that caffeine is present which might interfere chromatographically with hydrochlorothiazide As the spectra in Figure 40 on page 113 shows hydrochlorothiazide is best detecte...

Page 114: ...othiazide can be suppressed if caffeine is to be quantified In this case the wavelength is set to 204 nm and the reference wavelength to 260 nm Figure 41 on page 114 shows the chromatographic results of the peak suppression technique The trade off for this procedure is a loss in sensitivity The sample signal decreases by the absorbance at the reference wavelength relative to the signal wavelength ...

Page 115: ... or post column derivatization Specifying a signal ratio that is typical for the sample class is one way of selectively plotting only those peaks that are of interest The signal output remains at zero so long as the ratio is out of the user specified ratio range When the ratio falls within the range the signal output corresponds to the normal absorbance giving single clear peaks on a flat baseline...

Page 116: ...ier criterion and therefore the output was set to zero The characteristic wavelengths 249 nm λ1 and 224 nm λ2 were found from the spectra shown in Figure 42 on page 115 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 43 on page 116 The others were not plott...

Page 117: ...s Overview of the Module s Indicators and Test Functions 118 Status Indicators 119 Power Supply Indicator 119 Module Status Indicator 120 User Interfaces 121 Agilent Lab Advisor Software 122 This chapter gives an overview about the troubleshooting and diagnostic features and the different user interfaces ...

Page 118: ...nterface For each message a short description of the failure a list of probable causes of the problem and a list of suggested actions to fix the problem are provided see Error Information on page 123 Test Functions A series of test functions are available for troubleshooting and operational verification after exchanging internal components see Test Functions on page 143 Wavelength Verification Rec...

Page 119: ...ont of the module The lower left indicates the power supply status the upper right indicates the module status Figure 44 Location of Status Indicators Power Supply Indicator The power supply indicator is integrated into the main power switch When the indicator is illuminated green the power is ON LQH SRZHU VZLWFK ZLWK JUHHQ OLJKW 6WDWXV LQGLFDWRU JUHHQ HOORZ UHG ...

Page 120: ...tus indicator is red An error condition indicates the module has detected an internal problem which affects correct operation of the module Usually an error condition requires attention e g leak defective internal components An error condition always interrupts the analysis If the error occurs during analysis it is propagated within the LC system i e a red LED may indicate a problem of a different...

Page 121: ...tation In future a user interface may not show the Diagnostics Tests anymore Then the Agilent Diagnostic Software must be used instead The Agilent ChemStation may not include any maintenance test functions Table 18 Test Functions avaible vs User Interface Test Diagnostic Software ChemStation Instant Pilot G4208A Selftest Yes Yes No Filter Yes Yes No Slit Yes Yes No D A Converter Yes Yes No Test Ch...

Page 122: ...iagnostic capabilities calibration procedures and maintenance routines for all the maintenance routines The Agilent Lab Advisor software also allows users to monitor the status of their LC instruments The Early Maintenance Feedback EMF feature helps to carry out preventive maintenance In addition users can generate a status report for each individual LC instrument The tests and diagnostic features...

Page 123: ...Sensor Short 130 Fan Failed 130 Leak 131 Additional Information 132 Open Cover 133 Cover Violation 133 Detector Error Messages 134 Visible Lamp Current 134 Visible Lamp Voltage 134 Diode Current Leakage 135 UV Lamp Current 135 UV Lamp Voltage 136 UV Ignition Failed 136 UV Heater Current 137 Calibration Values Invalid 137 Holmium Oxide Test Failed 138 Illegal Temperature Value from Sensor on Main B...

Page 124: ...re Heater at fan assembly failed 140 Heater Power At Limit 140 DSP Not Running 141 No Run Data Available In Device 141 Instrument Logbook 142 This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions ...

Page 125: ... notification all LEDs get red and the run will be stopped Depending on the module type this stop is implemented differently For example for a pump the flow will be stopped for safety reasons For a detector the lamp will stay on in order to avoid equilibration time Depending on the error type the next run can only be started if the error has been resolved for example liquid from a leak has been dr...

Page 126: ...d Probable cause Suggested actions 1 The analysis was completed successfully and the timeout function switched off the module as requested Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required 2 A not ready condition was present during a sequence or multiple injection run for a period longer than the timeout threshold Check the logbook for the...

Page 127: ...minute the error message is generated Probable cause Suggested actions 1 Leak detected in another module with a CAN connection to the system Fix the leak in the external instrument before restarting the module 2 Leak detected in an external instrument with a remote connection to the system Fix the leak in the external instrument before restarting the module 3 Shut down in an external instrument wi...

Page 128: ...cools the leak sensor causing the leak sensor current to change within defined limits If the current increases above the upper limit the error message is generated Probable cause Suggested actions 1 CAN cable disconnected Ensure all the CAN cables are connected correctly Ensure all CAN cables are installed correctly 2 Defective CAN cable Exchange the CAN cable 3 Defective main board in another mod...

Page 129: ...pen circuit The resistance across the temperature compensation sensor NTC on the main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor increases above the upper limit the error message is generated Probable cause Suggested actions 1 Leak sensor not connected to the main b...

Page 130: ...fan in the module has failed The hall sensor on the fan shaft is used by the main board to monitor the fan speed If the fan speed falls below a certain limit for a certain length of time the error message is generated This limit is given by 2 revolutions second for longer than 5 seconds Depending on the module assemblies e g the lamp in the detector are turned off to assure that the module does no...

Page 131: ...ompensation sensor are used by the leak algorithm to determine whether a leak is present 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 main board Probable cause Suggested actions 1 Loose fittings Ensure all fittings are tight 2 Broken capillary Exchange defective capillaries 3 Leaking flo...

Page 132: ...h eventually terminates in the leak pan of the bottom module of the stack the detector With normal injection volumes and run times the output of port 4 is small and evaporates right in the sampler leak pan However the output of port 4 is significant and a substantial volume of ejected mobile phase reaches the detector leak pan There are two possible fixes Select the one which is most convenient 1 ...

Page 133: ...ted Cover Violation Error ID 7461 The top foam has been removed The sensor on the main board detects when the top foam is in place If the foam is removed while the lamps are on or if an attempt is made to switch on for example the lamps with the foam removed the lamps are switched off and the error message is generated Probable cause Suggested actions 1 The top foam was removed during operation Pl...

Page 134: ...ally monitors the voltage across the lamp during operation If the lamp voltage falls below the lower limit the error message is generated Probable cause Suggested actions 1 Lamp disconnected Ensure the visible lamp connector is seated firmly 2 Defective visible lamp Exchange the visible lamp 3 Defective connector or cable Please contact your Agilent service representative 4 Defective power supply ...

Page 135: ...n by the lamp during operation If the anode current falls below the lower current limit the error message is generated Probable cause Suggested actions 1 Defective PDA optical unit Please contact your Agilent service representative 2 Defective connector or cable Please contact your Agilent service representative Probable cause Suggested actions 1 Lamp disconnected Ensure the UV lamp connector is s...

Page 136: ... the error message is generated Probable cause Suggested actions 1 Defective UV lamp or non Agilent lamp Exchange the UV lamp 2 Defective detector main board Please contact your Agilent service representative 3 Defective power supply Please contact your Agilent service representative Probable cause Suggested actions 1 Lamp too hot Hot gas discharge lamps may not ignite as easily as cold lamps Swit...

Page 137: ... if the calibration data are valid If the data are invalid or cannot be read from the spectrometer ROM the error message is generated Probable cause Suggested actions 1 Lamp disconnected Ensure the UV lamp is connected 2 Ignition started without the top foam in place Please contact your Agilent service representative 3 Defective UV lamp or non Agilent lamp Exchange the UV lamp 4 Defective detector...

Page 138: ...1 Lamps switched off Ensure the lamps are switched on 2 Defective or dirty flow cell Ensure the flow cell is inserted correctly and is free from contamination cell windows buffers etc 3 Defective filter assembly Please contact your Agilent service representative 4 Defective achromat assembly Please contact your Agilent service representative 5 Defective PDA optical unit Please contact your Agilent...

Page 139: ...or your detector to operate correctly has been lost During calibration of the detector the calibration values are stored in ROM If no data is available in the spectrometer ROM the error message is generated Probable cause Suggested actions 1 The temperature sensor is defect Replace the cable to the main board Please contact your Agilent service representative 2 Detector is exposed to illegal ambie...

Page 140: ...vailable power of the heater reached either the upper or lower limit This event is sent only once per run The parameter determines which limit has been hit 0 means upper power limit hit excessive ambient temperature drop 1 means lower power limit hit excessive ambient temperature increase Probable cause Suggested actions 1 Defective connector or cable Please contact your Agilent service representa...

Page 141: ...takes longer and the detector uses special settings e g full data rate at 80 Hz plus full spectra plus all signals during data buffering Probable cause Suggested actions 1 Random communication error Switch the detector off and on again at the power switch If the error reoccurs Please contact your Agilent service representative 2 Defective detector main board Please contact your Agilent service rep...

Page 142: ...AD and MWD User Manual 7 Error Information Detector Error Messages Instrument Logbook Figure 45 Instrument Logbook NOTE The logbook does not indicate a communication loss power fail It just shows the recovering Power on Lamps on ...

Page 143: ...y Test 148 Test Evaluation 148 Holmium Oxide Test 151 Test Evaluation 151 ASTM Drift and Noise Test 154 Test Evaluation 154 Cell Test 156 Test Evaluation 156 Using the Built in Test Chromatogram 158 Procedure Using the Agilent Lab Advisor 158 Wavelength Verification and Calibration 160 This chapter describes the detector s built in test functions ...

Page 144: ... runs a series of individual tests and evaluates the results automatically The following tests are run Filter Test Slit Test Dark Current Test Intensity Test Wavelength Calibration Test Holmium Test Spectral Flatness Test ASTM Noise Test optional Figure 46 Self test For details refer to the individual tests on the following pages ...

Page 145: ... filter passes through the light path an absorbance maximum is seen Once the filter is in position the absorbance maximum of holmium oxide is determined Finally the filter is moved out of the light path During movement an additional absorbance maximum is expected as the edge of the filter passes through the light path The test passes successfully if the two maxima resulting from the edge of the fi...

Page 146: ...146 Agilent 1260 Infinity DAD and MWD User Manual 8 Test Functions Filter Test Figure 47 Filter Test Figure 48 Filter Test Signals ...

Page 147: ...mits Probable cause Suggested actions 1 Filter assembly lever and filter not installed Install the filter assembly 2 Defective filter motor Please contact your Agilent service representative Probable cause Suggested actions 1 Holmium oxide filter not installed Install the holmium oxide filter 2 Dirty or contaminated filter Exchange the holmium oxide filter ...

Page 148: ...orbing solvents the test should be done with water in the flow cell The shape of the intensity spectrum is primarily dependent on the lamp grating and diode array characteristics Therefore intensity spectra will differ slightly between instruments Figure 49 on page 149 shows a typical intensity test spectrum Test Evaluation The Agilent Lab Advisor ChemStation and Instant Pilot evaluate four spectr...

Page 149: ...sity Test Figure 50 Intensity Test Signal In case of low counts in one or more ranges start the testing with the comparison of values with flow cell vs flow cell removed Contaminations of the cell windows and or the lenses there are 3 between vis lamp and flow cell will reduce the light throughput ...

Page 150: ...w cell Run the cell test see Cell Test on page 156 If the test fails exchange the flow cell windows 3 Dirty or contaminated optical components achromat windows Clean optical components with alcohol and lint free cloth or replace the parts 4 Old or non Agilent lamp Exchange the lamp NOTE If the lamp fails in a single range there might be no reason to change the lamp if the application is not run in...

Page 151: ...ally To eliminate effects due to absorbing solvents the test should be done with water in the flow cell or with removed flow cell Test Evaluation Holmium Oxide Test Evaluation Limits The test is evaluated by the instrument and the measured maxima are displayed automatically The test fails if one or more of the maxima lies outside of the limits see Figure 51 on page 152 NOTE See also Declaration of...

Page 152: ...152 Agilent 1260 Infinity DAD and MWD User Manual 8 Test Functions Holmium Oxide Test Figure 51 Holmium Oxide Test Figure 52 Holmium Oxide Test Signal ...

Page 153: ...ration Recalibrate see Wavelength Verification and Calibration on page 160 and repeat the test 3 Dirty or contaminated flow cell Run the cell test see Cell Test on page 156 If the test fails exchange the flow cell windows 4 Dirty or contaminated optical components achromat windows Clean optical components with alcohol and lint free cloth or replace the parts see Intensity Test on page 148 5 Old or...

Page 154: ... ASTM noise test determines the detector noise over a period of 20 minutes The test is done with the flowcell removed so the test results are not influenced by solvent or pump effects On completion of the test the noise result is displayed automatically Test Evaluation Limit is 0 02 mAU Figure 53 ASTM Drift and Noise Test ...

Page 155: ...nd MWD User Manual 155 Test Functions 8 ASTM Drift and Noise Test Test Failed Probable cause Suggested actions 1 Insufficient lamp warm up time Allow lamp to warm up for at least 1 hour 2 Old or non Agilent lamp Exchange the lamp ...

Page 156: ...ted the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with water in the flow cell Test Evaluation Cell Test Evaluation The Agilent ChemStation calculates the intensity ratio automatically The intensity ratio typically between 0 5 and 0 7 for new standard flow cells and 0 1 to 0 3 for new mico ...

Page 157: ...o value NOTE This test can be used for the standard flow cells only The nano flow cells will give very low values due to their design Probable cause Suggested actions 1 Absorbing solvent or air bubble in flow cell Ensure the flow cell is filled with water and free from air bubbles 2 Dirty or contaminated flow cell Exchange the flow cell windows ...

Page 158: ...d either by means of a stop time or manually Procedure Using the Agilent Lab Advisor This procedure works for all Agilent 1200 Infinity detectors DAD MWD VWD FLD and RID The example figure is from the RID detector 1 Assure that the default LC method is loaded via the control software 2 Start the Agilent Lab Advisor software B 01 03 SP4 or later and open the detector s Tools selection 3 Open the te...

Page 159: ...uilt in Test Chromatogram 6 To start a test chromatogram enter in the command line STRT Figure 56 Test Chromatogram with Agilent Lab Advisor 7 To stop the test chromatogram enter in the command line STOP NOTE The test chromatogram is switched off automatically at the end of a run ...

Page 160: ...ate calibration than is possible with holmium oxide When verification is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with bubble free degassed HPLC water in the flow cell If a deviation is found and displayed it can be recalibrated by pressing Adjust The deviations are tracked in...

Page 161: ...alibration Wavelength calibration should be done after maintenance of the flow cell lamp exchange or after a major repair like processor board or optical unit exchange see also Replacing the Module s Firmware on page 203 After calibration the holmium oxide test see Figure 51 on page 152 provides verification of wavelength accuracy at three additional wavelengths ...

Page 162: ...162 Agilent 1260 Infinity DAD and MWD User Manual 8 Test Functions Wavelength Verification and Calibration ...

Page 163: ...176 Maintenance of High Pressure Flow Cell 180 Replacing Capillaries on a Standard Flow Cell 182 Replacing Capillaries on a Semi Micro and Micro Flow Cell 188 Nano Flow Cell Replacing or Cleaning 192 Nano Flow Cell Replacing or Cleaning 192 Cleaning or Exchanging the Holmium Oxide Filter 197 Correcting Leaks 200 Replacing Leak Handling System Parts 201 Replacing the CompactFlash Card G1315C G1365C...

Page 164: ...intenance Introduction to Maintenance Introduction to Maintenance The module is designed for easy maintenance Maintenance can be done from the front with module in place in the system stack NOTE There are no serviceable parts inside Do not open the module ...

Page 165: ...upplied by the vendor and follow good laboratory practice The volume of substances should be reduced to the minimum required for the analysis Do not operate the instrument in an explosive atmosphere WARNING Eye damage by detector light Eye damage may result from directly viewing the UV light produced by the lamp of the optical system used in this product Always turn the lamp of the optical system ...

Page 166: ... to the products failure to comply with procedures in Agilent product user guides or use of the products in violation of applicable laws rules or regulations Use your Agilent products only in the manner described in the Agilent product user guides CAUTION Safety standards for external equipment If you connect external equipment to the instrument make sure that you only use accessory units tested a...

Page 167: ...es not ignite An intensity test should be performed after replacement Flow cell exchange If application requires a different flow cell type A holmium or wavelength calibration test should be performed after replacement Flow cell parts Cleaning or exchange If leaking or if intensity drops due to contaminated flow cell windows A pressure tightness test should be done after repair Holmium oxide filte...

Page 168: ...ightly dampened with water or a solution of water and mild detergent Do not use an excessively damp cloth allowing liquid to drip into the module WARNING Liquid dripping into the electronic compartment of your module can cause shock hazard and damage the module Do not use an excessively damp cloth during cleaning Drain all solvent lines before opening any connections in the flow path ...

Page 169: ...iption 1 2140 0820 Longlife Deuterium lamp C with black cover and RFID tag 1 G1103 60001 Tungsten lamp Preparations Turn the lamp s off WARNING Eye damage by detector light Eye damage may result from directly viewing the light produced by the deuterium lamp used in this product Always turn the deuterium lamp off before removing it WARNING Injury by touching hot lamp If the detector has been in use...

Page 170: ...to the flow cell area 2 Disconnect lamp from the connector unscrew the Vis lamp left and or UV lamp right and remove the lamp Do not touch the glass bulb with your fingers 3 When replacing the Vis lamp assure that the Vis lamp is inserted as shown flat edge towards the deuterium lamp 4 Insert the lamp Fix the screws and reconnect the lamp to connector ...

Page 171: ...counter as described in the user interface documentation lamps with I D tag cannot be reset 7 Turn the lamp on and give the lamp 10 minutes to warm up 8 Perform a Wavelength Verification and Calibration on page 160 or a Holmium Oxide Test on page 151 to check the correct positioning of the UV lamp 9 Perform an Intensity Test on page 148 ...

Page 172: ... µL 120 bar 12 MPa 1 G1315 60015 High pressure flow cell 6 mm 1 7 µL 400 bar 40 MPa 1 Nano flow cell refer to Nano Flow Cell Replacing or Cleaning on page 192 1 G5615 60022 Standard flow cell bio inert 10 mm 13 µL 120 bar 12 MPa for MWD DAD includes Capillary Kit Flow Cells BIO p n G5615 68755 Preparations Turn the lamp s off Remove the front cover CAUTION Sample degradation and contamination of t...

Page 173: ...cell area 2 Open the flow cell cover NOTE 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 3 Disconnect the flow cell inlet capillary top and the waste tubing bottom from the unions 4 Loosen the thumb screw and remove the flow cell outlet capillary bottom with the union ...

Page 174: ...holder NOTE 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 Maintenance of Standard Semi Micro or Micro Flow Cell on page 176 or Maintenance of High Pressure Flow Cell on page 180 6 Insert the flow cell while pressing the flow cell holder ...

Page 175: ...w and Reconnect the waste tubing bottom to the union NOTE To check for leaks establish a flow and observe the flow cell outside of the cell compartment and all capillary connections Next Steps 8 Perform a Wavelength Verification and Calibration on page 160 or a Holmium Oxide Test on page 151 to check the correct positioning of the flow cell 9 Replace the front cover LQOHW RXWOHW ZDVWH WKXPEVFUHZ ...

Page 176: ... For parts see Standard Flow Cell on page 208 Semi Micro Flow Cell Parts on page 212 Micro Flow Cell on page 214 Preparations Turn the flow off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 172 NOTE The gaskets used in the standard and semi micro micro flow cell are different CAUTION Sample degradation and contamination of the instrument Metal parts in the flow pat...

Page 177: ...and must be on the light entrance side Verify that the gasket is positioned flat on the bottom and the light path is not blocked If you removed all individual parts from the window assembly refer to the figures in Standard Flow Cell on page 208 for the correct orientation of the parts 2 Use a tooth pick to remove the quartz window from the window assembly NOTE If the washers fall out of the window...

Page 178: ... or Micro Flow Cell 3 Orientation of Flow Cell Parts Standard Flow Cell on page 208 NOTE Gaskets 6 and 7 have different hole diameters 4 Assemble the washers and the window assembly in correct order 5 Correct orientation of spring washers 2 is required 6 Press the PTFE ring into the window assembly ...

Page 179: ...dy Next Steps 9 Using a 4 mm hex key tighten the window screw hand tight plus a quarter turn 10 Reconnect the capillaries see Exchanging a Flow Cell on page 172 11 Perform a leak test 12 Insert the flow cell 13 Replace the front cover 14 Perform a Wavelength Verification and Calibration on page 160 or a Holmium Oxide Test on page 151 to check the correct positioning of the flow cell R QRW PL WKH J...

Page 180: ...4 mm Tooth picks Parts required Description For parts see High Pressure Flow Cell on page 224 Preparations Turn the flow off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 172 NOTE All descriptions in this procedure are based on the default orientation of the cell as it is manufactured The heat exchanger capillary and the cell body can be fixed mirror symmetrically ...

Page 181: ...et only continue with step 8 Maintenance of Standard Semi Micro or Micro Flow Cell on page 176 2 Use a tooth pick to remove the quartz window from the window assembly NOTE If the washers fall out of the window assembly they must be inserted in the correct order with the PTFE ring to prevent any leaks from the flow cell window 3 Follow the procedure Maintenance of Standard Semi Micro or Micro Flow ...

Page 182: ...rations Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 172 NOTE All descriptions in this procedure are based on the default orientation of the cell as it is manufactured The heat exchanger capillary and the cell body can be fixed mirror symmetrically to have both capillaries routed to the bottom or to the top depending on the routing of the capil...

Page 183: ...r bio inert applications always use dedicated bio inert parts which can be identified by the bio inert symbol or other markers described in this manual Do not mix bio inert and non inert modules or parts in a bio inert system 1 Identify the inlet and outlet capillaries To replace the inlet capillary continue with step To replace the inlet capillary use a 4 mm wrench for the fitting 2 After replaci...

Page 184: ...tting 4 Unscrew the cell body from the heat exchanger and the heat exchanger from the clamp unit 5 Use a small flat screw driver to carefully lift off the I D tag Shown is the default orientation See Note at the beginning of this section 6 Unscrew the fixing screw and unwrap the inlet capillary from the grove in the flow cell body 6FUHZ QOHW FDSLOODU ZLWK KHDW H FKDQJHU ...

Page 185: ...Flow Cell 7 Take the new inlet capillary and bend it 90 about 35 mm from its end 8 Bend the capillary again by 90 as shown below 9 Insert the capillary into the hole between fixing screw and the inlet fitting 10 The capillary lays in the grove and should be tied around the body in the grove 5 times PP ...

Page 186: ...he grove 12 Carefully insert the I D tag into the new heat exchanger Shown is the default orientation See Note at the beginning of this section 13 Fix the heat exchanger to the clamp unit and the flow cell body to the heat exchanger 14 Fix the inlet capillary to the flow cell body handtight first Then do a 1 4 turn with a 4 mm wrench 6FUHZ QOHW FDSLOODU ZLWK KHDW H FKDQJHU ...

Page 187: ...le If required adjust with the holder screws Next Steps 16 Reconnect the capillaries see Exchanging a Flow Cell on page 172 17 Perform a leak test 18 Insert the flow cell 19 Replace the front cover 20 Perform a Wavelength Verification and Calibration on page 160 or a Holmium Oxide Test on page 151 to check the correct positioning of the flow cell ...

Page 188: ...s off Remove the front cover Remove the flow cell Exchanging a Flow Cell on page 172 NOTE All descriptions in this procedure are based on the default orientation of the cell as it is manufactured The heat exchanger capillary and the cell body can be fixed mirror symmetrically to have both capillaries routed to the bottom or to the top depending on the routing of the capillaries to the column NOTE ...

Page 189: ...entify the inlet and outlet capillaries 2 After replacing the outlet capillary fix it handtight first Then do a 1 4 turn with a 4 mm wrench 3 To replace the inlet capillary use a 4 mm wrench for the fitting 4 Unscrew the cell body from the heat exchanger and the heat exchanger from the clamp unit QOHW FDSLOODU 2XWOHW FDSLOODU ...

Page 190: ...n is the default orientation See Note at the beginning of this section 6 Carefully insert the I D tag into the new heat exchanger Shown is the default orientation See Note at the beginning of this section 7 Fix the new heat exchanger to the clamp unit and the heat exchanger to the cell body 8 Fix the inlet capillary to the flow cell body handtight first Then do a 1 4 turn with a 4 mm wrench ...

Page 191: ...vs hole If required adjust with the holder screws Next Steps 10 Reconnect the capillaries see Exchanging a Flow Cell on page 172 11 Perform a leak test 12 Insert the flow cell 13 Replace the front cover 14 Perform a Wavelength Verification and Calibration on page 160 or a Holmium Oxide Test on page 151 to check the correct positioning of the flow cell ...

Page 192: ...ch for capillary connections Parts required Description For parts identification refer to Nano Flow Cells on page 220 80 nL and 500 nL Preparations Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 172 NOTE For details refer to the technical note that comes with the nano flow cell kit NOTE The quartz block can be cleaned with alcohol DO NOT touch th...

Page 193: ...isconnect the capillaries from the capillary holder and remove the flow cell 2 Unscrew the cell body from the holder 3 Unscrew the capillaries from the flow cell DO NOT use the adapter at this time 4 Using for example a toothpick press on the plastic part and slide the quartz body out of the cell housing ...

Page 194: ...can be separated for cleaning purpose 6 This figure shows the correct holding of the quartz body and the cell seal assembly 7 Replace the cell seal assembly onto the quartz body Always use a new seal assembly to exclude damage during disassembling 8 Slide the quartz body completely into the cell body to the front stop use for example a toothpick ...

Page 195: ... connect the capillaries to the union holder Next Steps 12 Perform a leak test with the flow cell outside of the detector 13 If no leak is observed install the flow cell and you are ready to work 14 Make sure that the flow cell assembly is inserted correctly and fits perfectly in the optical unit especially when PEEK capillaries are used NOTE The cell body can be fitted in two positions to allow t...

Page 196: ...es a 4 mm wrench and with the Sealing Kit a special 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 The wrench has to be plugged into the adapter as shown in Figure 60 on page 196 UHQFK GDSWHU 2 127 SUHVV GRZQ PRUH WKDQ VKRZQ KHUH PD 1P ...

Page 197: ... see Exchanging a Flow Cell on page 172 NOTE See also Declaration of Conformity for HOX2 Filter on page 301 The glass tends to build a film on its surface even under normal environmental conditions This is a phenomenon which can be found also on the surface of several other glasses and has something to do with the composition of the glass There is no indication that the film has an influence on th...

Page 198: ...r 2 If not already in this position move the filter up 3 While releasing the holder with a screw driver at the top carefully remove the holmium oxide filter NOTE Do not scratch the holmium oxide filter The holmium oxide filter can be cleaned with alcohol and a lint free cloth 4 While releasing the holder with a screw driver carefully insert the holmium oxide filter ...

Page 199: ...de Filter 5 Replace the flow cell cover and fix the six screws Next Steps 6 Perform a holmium oxide test see Holmium Oxide Test on page 151 to check the proper function of the holmium oxide filter 7 Insert the flow cell see Exchanging a Flow Cell on page 172 8 Replace the front cover 9 Turn on the flow ...

Page 200: ...w cell area for leaks and correct if required Figure 61 Observing for Leaks 3 Replace the front cover When If a leakage has occurred in the flow cell area or at the heat exchanger or at the capillary connections Tools required p n Description Tissue Wrench 1 4 inch for capillary connections 5043 0915 Fitting mounting tool for bio inert capillaries Preparations Remove the front cover HDN SDQ HDN VH...

Page 201: ...ert the leak funnel with the tubing in its position 4 Insert the leak funnel into the leak funnel holder Figure 62 Replacing Leak Handling System Parts 5 Replace the front cover When If the parts are corroded or broken Tools required None Parts required p n Description 1 5041 8388 Leak funnel 1 5041 8389 Leak funnel holder 1 5062 2463 Corrugated tubing PP 6 5 mm id 5 m Preparations Remove the fron...

Page 202: ...ure 63 Replacing CompactFlash card When If defective Tools required None Parts required p n Description 1 01100 68700 CompactFlash Card Kit Preparations Turn the detector OFF and have access to the rear of the detector NOTE The G1315C and G1365C is equipped with a CompactFlash card This CompactFlash card is required for the operation of the detector data buffering DO NOT use other types of Compact...

Page 203: ...The installation of newer firmware might be necessary if a newer version solves problems of older versions or to keep all systems on the same validated revision The installation of older firmware might be necessary to keep all systems on the same validated revision or if a new module with newer firmware is added to a system or if third party control software requires a special version Tools requir...

Page 204: ...esident from the same revision set e g A 06 30 B 06 30 Compatibility with 1100 1200 series modules When using the G1315C D and G1365C D in a system all other modules must have firmware revision A 06 xx or B 01 02 or above main and resident Otherwise the communication will not work Compatibility with VSA Optical Introduced 08 2012 Firmware B 06 51 B 06 43 or B 06 26 or later depends on the used fir...

Page 205: ...of Maintenance Parts 206 Standard Flow Cell 208 Standard Flow Cell Bio inert 210 Semi Micro Flow Cell Parts 212 Micro Flow Cell 214 Prep Flow Cell SST 216 Prep Flow Cell Quartz 218 Nano Flow Cells 220 High Pressure Flow Cell 224 Accessory Kits 226 This chapter provides information on parts for maintenance ...

Page 206: ...Deuterium lamp C with black cover and RFID tag 9 G1103 60001 Tungsten lamp 10 5041 8388 Leak funnel 11 5041 8389 Leak funnel 12 5041 8387 Tube clip 13 5062 2463 Corrugated tubing PP 6 5 mm id 5 m 14 5062 2462 Tube PTFE 0 8 mm x 2 m re order 5 m 5181 1516 CAN cable Agilent module to module 0 5 m 5181 1519 CAN cable Agilent module to module 1 m G1369C or G1369 60012 Interface board LAN 5023 0203 Cro...

Page 207: ...Agilent 1260 Infinity DAD and MWD User Manual 207 Parts for Maintenance 10 Overview of Maintenance Parts Figure 64 Maintenance Parts ...

Page 208: ... 7 G1315 68710 Gasket FRONT PTFE 1 3 mm hole inlet side 12 pk 8 Window assembly comprises window screw spring washers compression washer window holder and quartz window G1315 87321 Capillary IN 0 17 mm 590 mm lg including heat exchanger 10 G1315 87302 Capillary OUT 0 17 mm 200 mm lg 11 G1315 84910 Clamp unit 0515 1056 Screw M 2 5 4 mm lg for cell body clamp 5022 2184 Union ZDV G1315 68712 Cell rep...

Page 209: ... Parts for Maintenance 10 Standard Flow Cell Figure 65 Standard Flow Cell Parts Figure 66 Orientation of Spring Washers NOTE Gaskets 6 and 7 have different hole diameters ZLQGRZ VFUHZ VSULQJ ZDVKHUV FRPSUHVVLRQ ZDVKHU ZLQGRZ KROGHU TXDUW ZLQGRZ DVNHW ...

Page 210: ...90 0921 Sapphire window 6 G1315 68711 Gasket BACK PTFE 2 3 mm hole outlet side 12 pk 7 G1315 68710 Gasket FRONT PTFE 1 3 mm hole inlet side 12 pk 8 Window assembly comprises window screw spring washers compression washer window holder and quartz window 9 G5615 87331 Capillary In 0 17 mm 590 mm lg including heat exchanger 10 G5615 87302 Capillary Out 0 17 mm 200 mm lg 11 G1315 84910 Clamp unit 0515...

Page 211: ...MWD User Manual 211 Parts for Maintenance 10 Standard Flow Cell Bio inert Figure 67 Standard Flow Cell Bio inert Figure 68 Orientation of Spring Washers ZLQGRZ VFUHZ VSULQJ ZDVKHUV FRPSUHVVLRQ ZDVKHU ZLQGRZ KROGHU TXDUW ZLQGRZ DVNHW ...

Page 212: ... 1 3 mm hole inlet side 12 pk 8 Window assembly comprises window screw spring washers compression washer window holder and quartz window 9 G1315 87319 Capillary IN 0 17 mm 310 mm lg including heat exchanger 10 G1315 87306 Capillary OUT 0 12 mm 200 mm lg 10 G1315 87302 Capillary OUT 0 17 mm 200 mm lg 11 G1315 84910 Clamp unit 0515 1056 Screw M 2 5 4 mm lg for cell body clamp 5022 2184 Union ZDV G13...

Page 213: ...s for Maintenance 10 Semi Micro Flow Cell Parts Figure 69 Semi Micro Flow Cell Parts Figure 70 Orientation of Spring Washers NOTE Gaskets 6 and 7 have different hole diameters ZLQGRZ VFUHZ VSULQJ ZDVKHUV FRPSUHVVLRQ ZDVKHU ZLQGRZ KROGHU TXDUW ZLQGRZ DVNHW ...

Page 214: ...le inlet side 12 pk 8 Window assembly comprises window screw spring washers compression washer window holder and quartz window 9 G1315 87339 DAD Heat Exchanger Capillary 310 mm 0 12 mm i d 10 G1315 87306 Capillary OUT 0 12 mm 200 mm lg 10 G1315 87302 Capillary OUT 0 17 mm 200 mm lg 11 G1315 84910 Clamp unit 0515 1056 Screw M 2 5 4 mm lg for cell body clamp 5022 2184 Union ZDV G1315 68713 Cell repa...

Page 215: ...215 Parts for Maintenance 10 Micro Flow Cell Figure 71 Micro Flow Cell Parts Figure 72 Orientation of Spring Washers NOTE Gaskets 6 and 7 have different hole diameters ZLQGRZ VFUHZ VSULQJ ZDVKHUV FRPSUHVVLRQ ZDVKHU ZLQGRZ KROGHU TXDUW ZLQGRZ DVNHW ...

Page 216: ...et side 12 pk 7 G1315 68710 Gasket FRONT PTFE 1 3 mm hole inlet side 12 pk 8 Window assembly comprises window screw spring washers compression washer window holder and quartz window 79883 68703 Window screw kit includes 2 quartz windows 2 compression washers 2 window holders 2 window screws and 10 washers G1315 68712 Cell repair kit STD includes window screw kit 4 mm hexagonal wrench and seal kit ...

Page 217: ...for Maintenance 10 Prep Flow Cell SST Figure 73 Prep Flow Cell SST Parts Figure 74 Orientation of Spring Washers LQOHW RXWOHW D NOTE Gaskets 6 and 7 have different hole diameters ZLQGRZ VFUHZ VSULQJ ZDVKHUV FRPSUHVVLRQ ZDVKHU ZLQGRZ KROGHU TXDUW ZLQGRZ DVNHW ...

Page 218: ... mm G1315 67302 PTFE tubing 80 cm length 0 5 mm i d o D 1 6 mm 2 0100 1516 Fitting male PEEK 2 pk 3 G1315 27705 Cell housing 4 G1315 84901 Clamp unit 5 G1315 84902 Handle for Clamp unit 6 0515 1056 Screw M 2 5 4 mm lg for cell body clamp 7 G1315 80004 Quartz body Prep Cell 0 3 mm 7 G1315 80003 Quartz body Prep Cell 0 06 mm NOTE The flow cell comes with two tubings 0 8 mm i d and one 0 5 mm i d so ...

Page 219: ...Agilent 1260 Infinity DAD and MWD User Manual 219 Parts for Maintenance 10 Prep Flow Cell Quartz Figure 75 Prep Flow Cell Quartz Parts RXWOHW LQOHW ...

Page 220: ...s 1 2 3 4 10 11 12 13 14 15 and 16 Nano flow cell kit 6 mm 80 nL 5 MPa G1315 68716 completely assembled includes items 1 2 3 4 10 11 12 13 14 15 and 16 Item p n Description 3 5063 6593 Fitting Screw for 4 mm wrench 4 Cell ferrules are factory installed 5 5065 4422 PEEK fitting 1 32 7 5063 6592 Litetouch ferrules LT 100 1 32 Ferrule and SS lock ring 8 5022 2146 Union Adjustment Tool 9 5022 2184 Uni...

Page 221: ...Agilent 1260 Infinity DAD and MWD User Manual 221 Parts for Maintenance 10 Nano Flow Cells Figure 76 Content of kits ...

Page 222: ...utlet 100 µm pre mounted to cell includes Outlet capillary 120 mm long 100 µm i d with pre fixed ferrules 4 and fitting 3 plus one PEEK Fitting FT 5 1 G1315 87323 PEEK coated fused silica capillary Inlet 50 µm alternative includes Inlet capillary 400 mm long 50 µm i d with pre fixed ferrules 4 and fittings 3 plus one PEEK Fitting FT 5 2 G1315 87328 PEEK coated fused silica capillary Outlet 50 µm a...

Page 223: ... 50 µm alternative includes Outlet capillary 120 mm long 50 µm i d with pre fixed ferrules 4 and fitting 3 plus one PEEK Fitting FT 5 1 G1315 87313 PEEK coated fused silica capillary Inlet 25 µm alternative includes Inlet capillary 200 mm long 25 µm i d with pre fixed ferrules 4 and fittings 3 plus one PEEK Fitting FT 5 2 G1315 87318 PEEK coated fused silica capillary Outlet 25 µm alternative incl...

Page 224: ...z window 4 79883 28802 Compression washer 5 5062 8553 Washer kit 10 pk 6 79883 22404 Window screw 7 G1315 87325 Capillary IN 0 12 mm 290 mm lg including heat exchanger 8 G1315 87306 Capillary OUT 0 12 mm 200 mm lg 9 G1315 84901 Clamp unit 0515 1056 Screw M 2 5 4 mm lg for cell body clamp G1315 87312 Capillary ST 0 12 mm x 150 mm S S G1315 87311 Capillary ST 0 17 mm x 380 mm S S 79883 68700 High pr...

Page 225: ...Agilent 1260 Infinity DAD and MWD User Manual 225 Parts for Maintenance 10 High Pressure Flow Cell Figure 77 High pressure flow cell parts ...

Page 226: ...PK Item p n Description 5063 6527 Tubing assembly i d 6 mm o d 9 mm 1 2 m to waste 1 5062 2462 Tube PTFE 0 8 mm x 2 m re order 5 m 2 0100 1516 Fitting male PEEK 2 pk 3 G1315 87311 Capillary ST 0 17 mm x 380 mm S S 4 5180 4108 Ferrule front 1 16 SST qty 2 re order pack of 10 5 5180 4114 Ferrule back 1 16 SST qty 2 re order pack of 10 6 5061 3303 Fitting 1 16 SST qty 2 re order pack of 10 G1315 8730...

Page 227: ...Agilent 1260 Infinity DAD and MWD User Manual 227 Parts for Maintenance 10 Accessory Kits Figure 78 Waste Tubing Parts Figure 79 Inlet Capillary Column Detector Parts 7KLV HQG LV SUH LQVWDOOHG ...

Page 228: ...228 Agilent 1260 Infinity DAD and MWD User Manual 10 Parts for Maintenance Accessory Kits ...

Page 229: ...ilent Technologies 11 Identifying Cables Cable Overview 230 Analog Cables 232 Remote Cables 234 BCD Cables 237 CAN LAN Cables 239 Agilent 1200 module to PC 240 This chapter provides information on cables used with the Agilent 1200 Infinity Series modules ...

Page 230: ...nt module to 3394 6 integrators 35900 60750 Agilent 35900A A D converter 01046 60105 Analog cable BNC to general purpose spade lugs p n Description 03394 60600 Agilent module to 3396A Series I integrators 3396 Series II 3395A integrator see details in section Remote Cables on page 234 03396 61010 Agilent module to 3396 Series III 3395B integrators 5061 3378 Remote Cable 01046 60201 Agilent module ...

Page 231: ...able shielded 3 m for point to point connection 5023 0202 Twisted pair network cable shielded 7 m for point to point connection p n Description G1530 60600 RS 232 cable 2 m RS232 61601 RS 232 cable 2 5 m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It s also called Null Modem Cable with full handshaking where the wiri...

Page 232: ... One end of these cables provides a BNC connector to be connected to Agilent modules The other end depends on the instrument to which connection is being made Agilent Module to 3394 6 Integrators p n 35900 60750 Pin 3394 6 Pin Agilent module Signal Name 1 Not connected 2 Shield Analog 3 Center Analog ...

Page 233: ...1 Analog Cables Agilent Module to BNC Connector Agilent Module to General Purpose p n 8120 1840 Pin BNC Pin Agilent module Signal Name Shield Shield Analog Center Center Analog p n 01046 60105 Pin Pin Agilent module Signal Name 1 Not connected 2 Black Analog 3 Red Analog ...

Page 234: ... Integrators Agilent Module to 3396 Series II 3395A Integrators Use the cable Agilent module to 3396A Series I integrators 03394 60600 and cut pin 5 on the integrator side Otherwise the integrator prints START not ready p n 03394 60600 Pin 3396A Pin Agilent module Signal Name Active TTL 9 1 White Digital ground NC 2 Brown Prepare run Low 3 3 Gray Start Low NC 4 Blue Shut down Low NC 5 Pink Not con...

Page 235: ... 3 Gray Start Low NC 4 Blue Shut down Low NC 5 Pink Not connected NC 6 Yellow Power on High 14 7 Red Ready High 4 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected p n 5061 3378 Pin 35900 A D Pin Agilent module Signal Name Active TTL 1 White 1 White Digital ground 2 Brown 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low 5 Pink 5 Pink Not connected 6 Yello...

Page 236: ...ilent Module to General Purpose p n 01046 60201 Wire Color Pin Agilent module Signal Name Active TTL White 1 Digital ground Brown 2 Prepare run Low Gray 3 Start Low Blue 4 Shut down Low Pink 5 Not connected Yellow 6 Power on High Red 7 Ready High Green 8 Stop Low Black 9 Start request Low ...

Page 237: ...ument to be connected to Agilent Module to General Purpose p n G1351 81600 Wire Color Pin Agilent module Signal Name BCD Digit Green 1 BCD 5 20 Violet 2 BCD 7 80 Blue 3 BCD 6 40 Yellow 4 BCD 4 10 Black 5 BCD 0 1 Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground Gray Gray pink 10 BCD 11 800 Red blue 11 BCD 10 400 White green 12 BCD 9 200 Brown green 13 BCD 8 100 not connected 14 ...

Page 238: ...tifying Cables BCD Cables Agilent Module to 3396 Integrators p n 03396 60560 Pin 3396 Pin Agilent module Signal Name BCD Digit 1 1 BCD 5 20 2 2 BCD 7 80 3 3 BCD 6 40 4 4 BCD 4 10 5 5 BCD0 1 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5 V Low ...

Page 239: ...nected to Agilent modules CAN or LAN connectors CAN Cables LAN Cables p n Description 5181 1516 CAN cable Agilent module to module 0 5 m 5181 1519 CAN cable Agilent module to module 1 m p n Description 5023 0203 Cross over network cable shielded 3 m for point to point connection 5023 0202 Twisted pair network cable shielded 7 m for point to point connection ...

Page 240: ...G1530 60600 RS 232 cable 2 m RS232 61601 RS 232 cable 2 5 m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It s also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8 m ...

Page 241: ...ctrical Connections 245 Serial Number Information ALL 246 Rear view of the module 246 Interfaces 247 Interfaces Overview 250 Setting the 8 bit Configuration Switch 254 Special Settings 256 Instrument Layout 258 Early Maintenance Feedback EMF 259 This chapter describes the detector in more detail on hardware and electronics ...

Page 242: ...operties are the complete communication capabilities CAN LAN and RS 232C memory management ability to update the firmware of the main system Main System Its properties are the complete communication capabilities CAN LAN and RS 232C memory management ability to update the firmware of the resident system In addition the main system comprises the instrument functions that are divided into common func...

Page 243: ... for the G1315A B DAD R the firmware revision for example A for G1315B or B for the G1315C DAD VVV is the revision number for example 102 is revision 1 02 XXX is the build number of the firmware For instructions on firmware updates refer to section Replacing Firmware in chapter Maintenance or use the documentation provided with the Firmware Update Tools Figure 80 Firmware Update Mechanism NOTE Upd...

Page 244: ...r their initial firmware revision For example a G1315C DAD SL cannot be downgraded below firmware revision B 01 02 or to a A xx xx Some modules can be re branded e g G1314C to G1314B to allow operation in specific control software environments In this case the feature set of the target type are use and the feature set of the original are lost After re branding e g from G1314B to G1314C the origina...

Page 245: ...epare and so on With the appropriate software the RS 232C connector may be used to control the module from a computer through a RS 232C connection This connector is activated and can be configured with the configuration switch The power input socket accepts a line voltage of 100 240 VAC 10 with a line frequency of 50 or 60 Hz Maximum power consumption varies by module There is no voltage selector ...

Page 246: ...labels provide the following information Rear view of the module Figure 81 Rear View of Detector CCXZZ00000 Format CC Country of manufacturing DE Germany JP Japan CN China X Alphabetic character A Z used by manufacturing ZZ Alpha numeric code 0 9 A Z where each combination unambiguously denotes a module there can be more than one code for the same module 00000 Serial number ...

Page 247: ...1312C Bin Pump VL 1376A Cap Pump G2226A Nano Pump G5611A Bio inert Quat Pump 2 Yes No Yes 1 Yes G4220A B Bin Pump G4204A Quat Pump 2 No Yes Yes No Yes CAN DC OUT for CAN slaves G1361A Prep Pump 2 Yes No Yes No Yes CAN DC OUT for CAN slaves Samplers G1329B ALS G2260A Prep ALS 2 Yes No Yes No Yes THERMOSTAT for G1330B K1330B G1364B FC PS G1364C FC AS G1364D FC μS G1367E HiP ALS K1367E HiP ALS Clinic...

Page 248: ... Yes G1321B FLD K1321B FLD Clinical Ed G1321C FLD 2 Yes No Yes 2 Yes G1362A RID 2 Yes No Yes 1 Yes G4280A ELSD No No No Yes Yes Yes EXT Contact AUTOZERO Others G1170A Valve Drive 2 No No No No No 1 G1316A C TCC K1316C TCC Clinical Ed 2 No No Yes No Yes G1322A DEG K1322A DEG Clinical Ed No No No No No Yes AUX G1379B DEG No No No Yes No Yes G4225A DEG K4225A DEG Clinical Ed No No No Yes No Yes Table...

Page 249: ...No No No No CAN DC OUT for CAN slaves 1 G4240A CHIP CUBE 2 Yes No Yes No Yes CAN DC OUT for CAN slaves THERMOSTAT for G1330A B NOT USED K1330B 1 Requires a HOST module with on board LAN e g G4212A or G4220A with minimum firmware B 06 40 or C 06 40 or with additional G1369C LAN Card Table 22 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD optional LAN on board RS 232 Analog APG Remote Sp...

Page 250: ...ware B 06 40 or later or with additional G1369C LAN Card RS 232C Serial The RS 232C connector is used to control the module from a computer through RS 232C connection using the appropriate software This connector can be configured with the configuration switch module at the rear of the module Refer to Communication Settings for RS 232C The RS 232C is designed as DCE data communication equipment wi...

Page 251: ...Signal Output The analog signal output can be distributed to a recording device For details refer to the description of the module s main board Table 23 RS 232C Connection Table Pin Direction Function 1 In DCD 2 In RxD 3 Out TxD 4 Out DTR 5 Ground 6 In DSR 7 Out RTS 8 In CTS 9 In RI QVWUXPHQW 3 0DOH HPDOH HPDOH 0DOH ...

Page 252: ...em s critical parts in case any module detects a serious problem To detect whether all participating modules are switched on or properly powered one line is defined to summarize the POWER ON state of all connected modules Control of analysis is maintained by signal readiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines In addition PREP...

Page 253: ...me controlled activities 4 SHUT DOWN L System has serious problem for example leak stops pump Receiver is any module capable to reduce safety risk 5 Not used 6 POWER ON H All modules connected to system are switched on Receiver is any module relying on operation of others 7 READY H System is ready for next analysis Receiver is any sequence controller 8 STOP L Request to reach system ready state as...

Page 254: ...rial communication protocol and instrument specific initialization procedures All modules with on board LAN Default is ALL switches DOWN best settings Bootp mode for LAN and 19200 baud 8 data bit 1 stop bit with no parity for RS 232 For specific LAN modes switches 3 8 must be set as required For boot test modes switches 1 2 must be UP plus required mode Figure 83 Location of Configuration Switch e...

Page 255: ...n board LAN Mode Function SW 1 SW 2 SW 3 SW 4 SW 5 SW 6 SW 7 SW 8 LAN 0 0 Link Configuration Init Mode Selection Auto negotiation 0 x x x x x 10 MBit half duplex 1 0 0 x x x 10 MBit full duplex 1 0 1 x x x 100 MBit half duplex 1 1 0 x x x 100 MBit full duplex 1 1 1 x x x Bootp x x x 0 0 0 Bootp Store x x x 0 0 1 Using Stored x x x 0 1 0 DHCP x x x 1 0 0 Using Default x x x 0 1 1 TEST 1 1 System NV...

Page 256: ...ain the instrument firmware stays in the resident mode It is not operable as a module It only uses basic functions of the operating system for example for communication In this mode the main firmware can be loaded using update utilities NOTE For explanation of Boot Resident System and Revert to Default Data Coldstart refer to Special Settings on page 256 NOTE The tables include both settings for m...

Page 257: ...witch settings and power the instrument up again a forced cold start has been completed CAUTION Loss of data Forced cold start erases all methods and data stored in the non volatile memory Exceptions are calibration settings diagnosis and repair log books which will not be erased Save your methods and data before executing a forced cold start Table 27 Forced Cold Start Settings On board LAN Mode S...

Page 258: ... is then housed in a metal inner cabinet which is enclosed by a plastic external cabinet The advantages of this packaging technology are virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations the pla...

Page 259: ...er interface when the limit is exceeded Some counters can be reset to zero after the required maintenance procedure Using the EMF Counters The user settable EMF limits for the EMF Counters enable the early maintenance feedback to be adapted to specific user requirements The useful maintenance cycle is dependent on the requirements for use Therefore the definition of the maximum limits need to be d...

Page 260: ...260 Agilent 1260 Infinity DAD and MWD User Manual 12 Hardware Information Early Maintenance Feedback EMF ...

Page 261: ...ation with BootP 273 About Agilent BootP Service 273 How BootP Service Works 274 Situation Cannot Establish LAN Communication 274 Installation of BootP Service 275 Two Methods to Determine the MAC Address 277 Assigning IP Addresses Using the Agilent BootP Service 278 Changing the IP Address of an Instrument Using the Agilent BootP Service 281 Storing the settings permanently with Bootp 283 Manual ...

Page 262: ...network device will have the same hardware address The MAC address can be found on a label at the rear of the module underneath the configuration switch see Figure 85 on page 262 Figure 84 MAC Label 2 Connect the instrument s LAN interface see Figure 85 on page 262 to the PC network card using a crossover network cable point to point or a hub or switch using a standard LAN cable Figure 85 Location...

Page 263: ... requesting the parameters from a network based DHCP Server using the so called Dynamic Host Configuration Protocol This mode requires a LAN onboard Module or a G1369C LAN Interface card see Setup DHCP on page 270 by manually setting the parameters using Telnet by manually setting the parameters using the Instant Pilot G4208A The LAN interface differentiates between several initialization modes Th...

Page 264: ...on Switch The module is shipped with all switches set to OFF as shown above NOTE To perform any LAN configuration SW1 and SW2 must be set to OFF Table 28 Factory Default Settings Initialization Init Mode Bootp all switches down For details see Initialization mode selection on page 265 Link Configuration speed and duplex mode determined by auto negotiation for details see Link configuration selecti...

Page 265: ...ameters obtained become the active parameters immediately They are not stored to the non volatile memory of the module Therefore the parameters are lost with the next power cycle of the module Figure 87 Bootp Principle Table 29 Initialization Mode Switches SW 6 SW 7 SW 8 Init Mode OFF OFF OFF Bootp OFF OFF ON Bootp Store OFF ON OFF Using Stored OFF ON ON Using Default ON OFF OFF DHCP 1 1 Requires ...

Page 266: ...Bootp In this case he starts the Bootp Server temporarily powers on the module using the initialization mode Bootp Store waits for the Bootp cycle to be completed closes the Bootp Server and powers off the module Then he selects the initialization mode Using Stored and powers on the module again From now on he is able to establish the TCP IP connection to the module with the parameters obtained in...

Page 267: ...inciple Using Default When Using Default is selected the factory default parameters are taken instead These parameters enable a TCP IP connection to the LAN interface without further configuration see Table 30 on page 267 Figure 90 Using Default Principle 1RQ 9RODWLOH 5 0 6WRUHG 3DUDPHWHU FWLYH 3DUDPHWHU FWLYH 3DUDPHWHU HIDXOW 3DUDPHWHU NOTE Using the default address in your local area network may...

Page 268: ...ry of the module He may then close the session select the initialization mode Using Stored power on again and establish the TCP IP connection using the new parameters When the module is wired to the PC directly e g using a cross over cable or a local hub separated from the local area network the user may simply keep the default parameters to establish the TCP IP connection NOTE In the Using Defaul...

Page 269: ...ately They are not stored to the non volatile memory of the card Besides requesting the network parameters the card also submits its hostname to the DHCP Server The hostname equals the MAC address of the card e g 0030d3177321 It is the DHCP server s responsibility to forward the hostname address information to the Domain Name Server The card does not offer any services for hostname resolution e g ...

Page 270: ...ot the MAC address can be found under Details in the LAN section Figure 92 LAN Setting on Instant Pilot 2 Set the Configuration Switch to DHCP either on the G1369C LAN Interface Card or the main board of above mentioned modules Software required The modules in the stack must have at least firmware from set A 06 34 and the above mentioned modules B 06 40 or above must from the same firmware set Tab...

Page 271: ... Control Software e g Agilent ChemStation Lab Advisor Firmware Update Tool and use MAC address as host name e g 0030d3177321 The LC system should become visible in the control software see Note in section General Information DHCP on page 269 Table 32 LC Modules inclusive 1120 1220 configuration switch at rear of the instru ment SW 6 SW 7 SW 8 Initialization Mode ON OFF OFF DHCP ...

Page 272: ...re itself for 10 or 100 Mbps half duplex operation For example when connected to a non negotiating 10 Mbps hub the LAN interface will be automatically set to operate at 10 Mbps half duplex If the module is not able to connect to the network through auto negotiation you can manually set the link operating mode using link configuration switches on the module Table 33 Link Configuration Switches SW 3...

Page 273: ...ddresses for Agilent instruments on a LAN The BootP service must be running TCP IP network protocol and cannot run a DHCP server NOTE All examples shown in this chapter will not work in your environment You need your own IP Subnet Mask and Gateway addresses NOTE Assure that the detector configuration switch is set properly The setting should be either BootP or BootP Store see Table 29 on page 265 ...

Page 274: ... powered on Powering down the instrument causes it to lose its IP address so the Agilent BootP Service must be running every time the instrument powers up If the Agilent BootP Service runs in the background the instrument will receive its IP address on power up The Agilent LAN Interface can be set to store the IP address and will not lose the IP address if power cycled Situation Cannot Establish L...

Page 275: ...utomatically click Cancel to stop it 4 Open Windows Explorer 5 Go to the BootP directory on the Agilent ChemStation DVD and double click BootPPackage msi 6 If necessary click the Agilent BootP Service icon in the task bar 7 The Welcome screen of the Agilent BootP Service Setup Wizard appears Click Next 8 The End User License Agreement screen appears Read the terms indicate acceptance then click Ne...

Page 276: ...n be used The default subnet mask is 255 255 255 0 The default gateway is 192 168 254 11 13 On the BootP Settings screen click OK The Agilent BootP Service Setup screen indicates completion 14 Click Finish to exit the Agilent BootP Service Setup screen 15 Remove the DVD from the drive This completes installation 16 Start BootP Service in the Windows services On the Windows desktop click right on C...

Page 277: ...mation from BootP 3 Click OK to save the values or Cancel to discard them The editing ends 4 After each modification of the BootP settings i e EditBootPSettings a stop or start of the BootP service is required for the BootP service to accept changes See Stopping the Agilent BootP Service on page 281 or Restarting the Agilent BootP Service on page 282 5 Uncheck the Do you want to log BootP requests...

Page 278: ...e 0010835675AC 4 The Error means the MAC address has not been assigned an IP address and the Tab File does not have this entry The MAC address is saved to the Tab File when an IP address is assigned 5 Close the log file before turning on another instrument 6 Uncheck the Do you want to log BootP requests box after configuring instruments to avoid having the logfile use up excessive disk space Addin...

Page 279: ...The Do you want to log BootP requests box must be unchecked when you have finished configuring instruments otherwise the log file will quickly fill up disk space 3 Click Edit BootP Addresses The Edit BootP Addresses screen appears 4 Click Add The Add BootP Entry screen appears Figure 95 Enable BootP logging ...

Page 280: ...ose 8 Exit BootP Settings by pressing OK 9 After each modification of the BootP settings i e EditBootPSettings a stop or start of the BootP service is required for the BootP service to accept changes See Stopping the Agilent BootP Service on page 281 or Restarting the Agilent BootP Service on page 282 10 Power cycle the Instrument OR If you changed the IP address power cycle the instrument for the...

Page 281: ...matically when your PC reboots To change Agilent BootP Service settings you must stop the service make the changes and then restart the service Stopping the Agilent BootP Service 1 From the Windows control panel select Administrative Tools Services The Services screen appears Figure 96 Windows Services screen 2 Right click Agilent BootP Service 3 Select Stop 4 Close the Services and Administrative...

Page 282: ...4 In the Edit BootP Addresses screen press Add to create a new entry or select an existing line from the table and press Modify or Delete to change the IP address comment subnet mask for example in the Tab File If you change the IP address it will be necessary to power cycle the instrument for the changes to take effect 5 Leave Edit BootP Addresses by pressing Close 6 Exit BootP Settings by pressi...

Page 283: ... If required modify the parameters for the module according to your needs using the existing configuration 5 Press OK to exit the Bootp Manager 6 Now turn on the module and view the Bootp Server window After some time the Agilent Bootp Service will display the request from the LAN interface The parameters are now stored permanently in the non volatile memory of the module 7 Close the Agilent Bootp...

Page 284: ...latile memory of the module It never affects the currently active parameters Therefore manual configuration can be done at any time A power cycle is mandatory to make the stored parameters become the active parameters given that the initialization mode selection switches are allowing it Figure 98 Manual Configuration Principle 7 1 7 6HVVLRQ RQWURO 0RGXOH 6WRUHG 3DUDPHWHU 1RQ 9RODWLOH 5 0 ...

Page 285: ...g on Windows START button and select Run Type cmd and press OK 2 Type the following at the system DOS prompt c telnet IP address or c telnet host name Figure 99 Telnet Starting a session where IP address may be the assigned address from a Bootp cycle a configuration session with the Handheld Controller or the default IP address see Configuration Switch on page 264 When the connection was establish...

Page 286: ... press Enter where parameter refers to the configuration parameter you are defining and value refers to the definitions you are assigning to that parameter Each parameter entry is followed by a carriage return Table 34 Telnet Commands Value Description displays syntax and descriptions of commands displays current LAN settings ip x x x x sets new ip address sm x x x x sets new subnet mask gw x x x ...

Page 287: ...de information about the LAN interface MAC address initialization mode Initialization mode is Using Stored active TCP IP settings TCP IP status here ready connected to PC with controller software e g Agilent ChemStation here not connected Figure 103 Telnet Change IP settings change of IP setting to Initialization mode is Using Stored active TCP IP settings stored TCP IP settings in non volatile me...

Page 288: ...ng the configuration parameters type exit and press Enter to exit with storing parameters Figure 104 Closing the Telnet Session NOTE If the Initialization Mode Switch is changed now to Using Stored mode the instrument will take the stored settings when the module is re booted In the example above it would be 134 40 27 99 ...

Page 289: ...the module to the network the Instant Pilot G4208A can be used 1 From the Welcome screen press the More button 2 Select Configure 3 Press the DAD button 4 Scroll down to the LAN settings Figure 105 Instant Pilot LAN Configuration 5 Press the Edit button only visible if not in Edit mode perform the required changes and press the Done button 6 Leave the screen by clicking Exit ...

Page 290: ...290 Agilent 1260 Infinity DAD and MWD User Manual 13 LAN Configuration Manual Configuration ...

Page 291: ...Interference 296 Sound Emission 297 UV Radiation 298 Solvent Information 299 Declaration of Conformity for HOX2 Filter 301 Installation of Stainless Steel Cladded PEEK Capillaries 302 First Step Finger tight Fitting 303 Second Step Installation to Connector 303 Removing Capillaries 307 Agilent Technologies on Internet 308 This chapter provides addition information on safety legal and web ...

Page 292: ... and has been manufactured and tested according to international safety standards Operation Before applying power comply with the installation section Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a prote...

Page 293: ...d involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or ...

Page 294: ...s eye damage may result from directly viewing the light produced by the deuterium lamp used in this product The apparatus is marked with this symbol when hot surfaces are available and the user should not touch it when heated up WARNING A WARNING alerts you to situations that could cause physical injury or death Do not proceed beyond a warning until you have fully understood and met the indicated ...

Page 295: ...n all Electric and Electronic appliances from 13 August 2005 NOTE This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex I this product is classed as a Monitoring and Control in...

Page 296: ...nt 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 297: ...aration 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 At Operator Position Normal Operation According to ISO 7779 1988 EN 27779 1991 Type Test ...

Page 298: ...it Values according to the American Conference of Governmental Industrial Hygienists Typically the radiation values are much smaller than these limits NOTE This information is only valid for UV lamps without cover e g 2140 0590 and 2140 0813 Table 36 UV Radiation Limits Exposure day Effective Irradiance 8 hours 0 1 µW cm2 10 minutes 5 0 µW cm2 Table 37 UV Radiation Typical Values Position Effectiv...

Page 299: ... the use of solvents Brown glass ware can avoid growth of algae Small particles can permanently block capillaries and valves Therefore always filter solvents through 0 4 μm filters Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric...

Page 300: ...tographic 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 Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride with 2 propanol or THF ...

Page 301: ...Agilent 1260 Infinity DAD and MWD User Manual 301 Appendix 14 Declaration of Conformity for HOX2 Filter Declaration of Conformity for HOX2 Filter ...

Page 302: ...or is soft or hard Compared with hard connectors a greater tightening angle is required for soft connectors to achieve same torque whether the capillary is installed for the first time or subsequent times For the first time a greater tightening angle needs to be applied The installation consists of two steps In the first step the fitting is installed finger tight without using tools Finger tight m...

Page 303: ...ommended range in which the fitting is tight Staying below this range could create a leak either a visible one or a micro leak potentially biasing measurement results Exceeding the recommended range could damage the capillary Alternatively a torque wrench may be used The target torque for all connections is about 0 7 Nm When using a torque wrench read instructions for that tool carefully as wrong ...

Page 304: ... second and subsequent times again start from the finger tight position which is not necessarily a vertical wrench position and rotate the wrench by 90 135 Staying below 90 grey arrow could be insufficiently tight more than 135 red arrow could damage the capillary Second Step Installation to Soft Connectors Use this procedure for soft connectors which are typically made from PEEK These are the fol...

Page 305: ...hich does not necessarily need to be a vertical wrench position and rotate the wrench by 180 210 Staying below 180 grey arrow will not be sufficiently tight more than 210 red arrow could damage the capillary Second and subsequent installations of a capillary to a soft connector 1 When tightening the fitting for the second and subsequent times again start from the finger tight position which is not...

Page 306: ...el Cladded PEEK Capillaries Summary for Second Step Table 38 Summary for second step 2ndStep First installation Subsequent installations Hard connectors Soft connectors SRVVLEO OHDN UHFRPPHQGHG UDQJH SRVVLEO OHDN UHFRPPHQGHG UDQJH UHFRPPHQGHG UDQJH SRVVLEO OHDN SRVVLEO OHDN UHFRPPHQGHG UDQJH ...

Page 307: ...pand to the shape of the connector where the capillary is installed If the capillary is removed this may become visible as a small step In such cases do not try to pull the fitting from the capillary as this can destroy the front part of the capillary Instead carefully pull it to the rear During installation of the capillary the fitting will end up in the correct position Figure 106 Capillary fitt...

Page 308: ...ty DAD and MWD User Manual 14 Appendix Agilent Technologies on Internet Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com ...

Page 309: ...281 Bootp Store 266 automatic configuration 273 initialization modes 265 storing the settings permanently 283 using default 267 using stored 267 C cable analog 232 BCD 237 CAN 239 connecting APG remote 43 connecting CAN 43 connecting LAN 43 connecting the ChemStation 43 connecting the power 43 LAN 239 remote 234 RS 232 240 cables analog 230 BCD 230 CAN 231 LAN 231 overview 230 remote 230 RS 232 23...

Page 310: ...y and maintenance 35 26 29 32 filter test 145 firmware description 242 main system 242 resident system 242 update tool 243 updates 243 203 203 upgade downgrade 203 upgrade downgrade 203 flow cell correction factors 104 installation 51 solvent information 299 specifications 34 25 28 31 support windows 12 test 156 frequency range 23 G general error messages 126 GLP features 26 29 32 35 grating 12 13...

Page 311: ...ifications 36 non operating altitude 23 non operating temperature 23 O operating Altitude 23 operating temperature 23 optimization detector performance 100 for sensitivity selectivity linearity dispersion 103 how to get the best performance 100 margins for negative absorbance 112 of selectivity 113 of the system 67 overview 101 peak width 105 sample and reference wavelength 107 slit width 110 spec...

Page 312: ...30 programmable slit width 33 24 27 30 safety and maintenance 35 26 29 32 wavelength accuracy 33 24 27 30 wavelength bunching 33 24 27 30 wavelength range 33 24 27 30 spectra acquisition 112 spectrograph diodes per nm 12 stack configuration front view 42 rear view 43 status indicator 120 storing the settings permanently 283 suppression quantifying 113 T TCP IP parameter configuration 263 telnet co...

Page 313: ......

Page 314: ... Book This manual contains technical reference information about the Agilent 1260 Infinity diode array and multiple wavlength detectors G1315C D and G1365C D The manual describes the following introcduction and specifications installation using and optimizing troubleshooting and diagnose maintenance parts identification safety and related information ...

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