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G1314-90013 - Agilent Technologies

1. Window VWD A Absorbance at 254 nm x axis 15 Hmn Type acquired y axis range 1 mau draw zero line auto y adjust Offset 10 ds at 254 nm m Method Settings Use method settings Apply to Method Cancel Help Figure 17 Edit Signal Plot Window Agilent 1260 Infinity VWD User Manual 57 4 Using the Detector Setting up an Analysis The Online Plot Figure 18 on page 58 shows both the pump pressure and the detector absorbance signals Pressing Adjust the signals can be reset to the offset value and Balance would do a balance on the detector i j Online Plot Quatemary Pump Pressure Figure 18 Online Plot Window 13 If both baselines are stable set the Y range for the detector signal to 100 mAU If you start with a new UV lamp for the first time the lamp may show initial drift for some NOTE A time burn in effect 58 Agilent 1260 Infinity VWD User Manual Using the Detector 4 tting up an Anal 14 Select the menu item RunControl gt Sample Info and enter information about this application Figure 19 on page 59 Press OK to leave this screen Sample Info Offline Data Analysis x Operator Name wolfgang Data File Resume Injection Run Sequence F6 Pause Sequence Resume Sequence Path JE CHEMSTATION 2 DATAS z Subdirectory ISOTEST Stop RunjInj
2. Table 23 Data Bit Settings without on board LAN Switch 6 Data Word Size 0 1 7 Bit Communication 8 Bit Communication Table 24 Parity Settings without on board LAN Switches 7 8 0 0 0 1 1 1 Parity No Parity Odd Parity Even Parity One start bit and one stop bit are always used not selectable Per default the module will turn into 19200 baud 8 data bit with no parity Agilent 1260 Infinity VWD User Manual 177 12 Hardware Information Special Settings The special settings are required for specific actions normally in a service case Boot Resident Firmware update procedures may require this mode in case of firmware loading errors main firmware part If you use the following switch settings and power the instrument up again 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 Table25 Boot Resident Settings without on board LAN Mode Select SW1 sw Sw3 swa4 SW5 SW6 SW7 SW8 No LAN TEST BOOT 1 1 0 0 1 0 0 0 Forced Cold Start A forced cold start can be used to bring the module into a defined mode with default parameter settings CAUTION Loss of data Forced cold start erases all methods and data stored in the non volatile memory Exceptions are calibration s
3. DGCALOG1 M DGCALOQ2M File RunControl Instrument Method Sequence View Abort Help Gg Gg methods Lip ed oer cw Sequences iggy led oer ics ll Method and Run Control n a 33 53 B 3 cd od Hag C CHEM32 2 METHODS al N m A D DEF ICM Gj sequence DEF LS E W BATCH M Sane SmO 2 QI DEMOCALI M QI DEMOCALZ M 1 QI DGALSTST M QI DGCALAS M vWD QI DGCALOQ1 M 9 QJ DGCALOQ2 M QI DGCALOQ3 M QI DGCALOQ4 M QJ DGCALOQS M QI DGCALOQS M DEFAULT D QJ DCALPS M QJ DecHPTST M QI DGCPTEST M QJ DeFLDTST M QI DGLEAKT M QI DGNOISE M QI DGNPTEST M QI DGTHMTST M QJ DGYWDDC M E Adata QJ ISOCRA M QI ISOPLOT M no Details E 1 1 GB free Figure 14 Loading Default LC Method 54 Agilent 1260 Infinity VWD User Manual Using the Detector 4 Setting up an Analysis 9 Click on the module icons Figure 15 on page 55 and open the Setup of these modules Figure 16 on page 56 shows the detector settings do not change the detector parameters at this time EE i i B l a E i W Method DET M ig Sequence pees EMF MEM SIX DEFAULT D Pa Online Spectra 8 Not Ready Information Help E Adata E 1 1 GB free Figure 15 Open the module menu 10 Enter the pump parameters mentioned under Table 8 on page 49 Agilent 1260 Infinity VWD User Manual 55 4 Using the Detector Setting up an Analysi
4. ez p Leak plane Waste outlet Leak sensor assembly Figure 39 Drying the Leak Sensor 128 Agilent 1260 Infinity VWD User Manual Replacing Leak Handling lt Replacing Leak Handling System Parts When Tools required Parts required Leak funnel holder Leak funnel Leak tubing Leak plan Waste outlet Leak sensor assembly Agilent 1260 Infinity VWD User Manual If the parts are corroded or broken None p n 1 5041 8389 1 5061 3356 1 5062 2463 1 2 3 4 5 6 7 Description Leak funnel holder Leak funnel Corrugated tubing PP 6 5 mm id 5m Pull the leak funnel out of the leak funnel holder Pull the leak funnel with the tubing out of its location Replace the leak funnel and or the tubing Insert the leak funnel with the tubing in its position Insert the leak funnel into the leak funnel holder Replace the front cover Maintenance 9 em Parts Remove the front cover to have access to the leak handling system E Figure 40 Replacing Waste Handling System Parts 129 9 Maintenance Replacing the Interface Board When When defective or for installation of the board or for all repairs inside the detector Parts required p n Description 1 G1351 68701 Interface board BCD with external contacts and BCD outputs OR 1 G1369B or Interface board LAN G1369 60002 OR 1 G1369C or Interface board LAN G1369 60012 1 Insta
5. Agilent Technologies Notices Agilent Technologies Inc 2011 2012 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 61314 90013 Rev B Edition 05 2012 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn This product may be used as a com ponent of an in vitro diagnostic sys tem if the system is registered with the appropriate authorities and com plies with the relevant regulations Otherwise it is intended only for gen eral laboratory use Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance of this document or of any information contained herein Should Agilent and the user have a separate w
6. Table 18 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 Instrument PC DCD 1 1 DCD RX 2 uu 2 RX TX 3 A 3 TX DTR 4 a 4 DTR GND 5 y 5 GND DSR 6 6 DSR RTS 7 X 7 RTS CTS 8 8 CTS RI 9 9 RI DB9 DB9 DB9 DB9 Male Female Female Male Figure 50 RS 232 Cable Analog 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 Agilent 1260 Infinity VWD User Manual Hardware Information 12 APG Remote The APG Remote connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features as common shut down prepare and so on Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements The subminiature D connector is used The module provides one remote connector which is inputs outputs wired or technique To provide maximum safety within a distributed analysis system one line is dedicated to SHUT DOWN the system 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 r
7. G5664A Bio inert FC AS G5667A Bio inert Autosampler G4226A ALS 2 Yes No Yes No Yes Detectors G1314B VWD VL 2 Yes No Yes 1 Yes G1314C VWD VL G1314E F VWD 2 No Yes Yes 1 Yes G4212A B DAD 2 No Yes Yes 1 Yes Agilent 1260 Infinity VWD User Manual 169 12 Hardware Information Table 17 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD LAN RS 232 Analog APG Special optional on board Remote G1315C DAD VL 2 No Yes Yes 2 Yes G1365C MWD G1315D DAD VL G1365D MWD VL G1321B FLD 2 Yes No Yes 1 Yes G1362A RID G4280A ELSD No No No Yes Yes Yes EXT Contact AUTOZERO Others G1170A Valve Drive 2 No No No No No 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 G1316A C TCC 2 No No Yes No Yes G1322A DEG No No No No No Yes AUX G1379B DEG No No No Yes No No AUX G4227A Flex Cube 2 No No No No No G4240A CHIP CUBE 2 Yes No Yes No Yes CAN DC OUT for CAN slaves THERMOSTAT for G1330A B NOT USED The detector DAD MWD FLD VWD RID is the preferred access point for control via LAN The inter module communication is done via CAN CAN connectors as interface to other modules LAN connector as interface to the control software RS 232C as interface to a computer REMOTE connector as interface to other Agilent products Analog output connector s for signal output 170 Agilent 1260 Infinity VWD User Manu
8. mau Bat 190 f vo nm Figure 22 Online Spectra Window 2 Change the absorbance and wavelength range according your needs 62 Agilent 1260 Infinity VWD User Manual Using the Detector 4 Scanning with the VWD Set up a run Start a run 3 While running on the baseline select from the menu Instrument gt More VWD Blank Scan A background scan is stored in the memory System 2 online Method amp Run Control Fie RunControl Method Sequence View Abort Help Step 1 Blank Scan scan of the background solvent is EN TETWD Signals NEN stored in the memory as Een Li E Step 2 Sample Scan scan of the peak of interest is Mora ven ea taken while the peak stays in the flow cell stop flow Snapshot igurati condition ggi ere System On Online Spectrum Sample Scan minus Blank Scan System Off dil BATCH KA x SA Esk DEF_L Revisions amp Serial s E DGNOI Columns iL INSTPE BL Loapr Configure 1100 1200 Access S 2 ml min 4 When the peak of interest enters the flow cell stop the flow set flow rate to zero or open the purge valve and wait a few moments to stabilize the concentration Turning off the pump would stop the run and no access to the sample scan is possible 5 Select from the menu Instrument gt More VWD gt Sample Scan A sample scan is taken in the range defined under Special Setpoints on page 65 and the Online Spectra window see
9. 3 Defective or non Agilent lamp Exchange the lamp 4 Defective main board Please contact your Agilent service representative 5 Defective power supply Please contact your Agilent service representative UV lamp no voltage Error ID 7451 The lamp anode voltage is missing The processor continually monitors the anode voltage across the lamp during operation If the anode voltage falls below the lower limit the error message is generated Agilent 1260 Infinity VWD User Manual Probable cause 1 Defective or non Agilent lamp 2 Defective power supply 3 Defective main board Ignition Failed Error ID 7452 Error Information 7 Suggested actions Exchange the lamp Please contact your Agilent service representative Please contact your Agilent service representative The lamp failed to ignite The processor monitors the lamp current during the ignition cycle If the lamp current does not rise above the lower limit within 2 5 s the error message is generated Probable cause 1 Lamp disconnected 2 Defective or non Agilent lamp 3 Defective power supply 4 Defective main board Agilent 1260 Infinity VWD User Manual Suggested actions Ensure the lamp is connected Exchange the lamp Please contact your Agilent service representative Please contact your Agilent service representative 91 7 92 Error Information No heater current Error ID 7453 The lamp heater current in
10. Method DEF_LC M ag Sequence DEF LC S EMF Sante SO u DEFAULT D E datas E 1 1 GB free 52 Kx E mid omg Ma AL E BI O Lon Jat no Details had Tr 10 T 5 Figure 12 Turning on the HPLC Module Agilent 1260 Infinity VWD User Manual Using the Detector 4 5 Purge the pump For more information Priming and Purging the System on page 46 6 Allow the detector to warm up of at least 60 minutes to provide a stable baseline see example in Figure 13 on page 53 VWD1 A Wavelength 254 nm LAMPON WW_LAMPON2 D 02 0 4 0 8 0 8 r T f T r 10 20 30 40 50 60 min Figure 13 Stabilization of Baseline 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 7 For the isocratic pump fill the solvent bottle with the mixture of HPLC grade bi distilled water 80 and acetonitrile 70 For binary and quaternary pumps you can use separate bottles Agilent 1260 Infinity VWD User Manual 53 4 Using the Detector Setting up an Analysis 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 Agilent 1200 Infinity Series modules zjx DEF_LC M c chem3252 methods uum
11. start stop common shut down prepare 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 on your module because the power supply has wide ranging capability There are no externally accessible fuses because automatic electronic fuses are implemented in the power supply Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations 166 Agilent 1260 Infinity VWD User Manual Hardware Information 12 Serial Number Information ALL Serial Number Information 1260 Infinity The serial number information on the instrument labels provide the following information CCXZZ00000 CC ZZ 00000 Format Country of manufacturing DE Germany JP Japan CN China Alphabetic character A Z used by manufacturing 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 Serial number Serial Number Information 1200 Series and 1290 Infinity The serial number information on the instrument labels provide the
12. through a lens a filter assembly an entrance slit a spherical mirror M1 a grating a second spherical mirror M2 a beam splitter and finally through a flow cell to the sample diode The beam through the flow cell is absorbed depending on the solutions in the cell in which UV absorption takes place and the intensity is converted to an electrical signal by means of the sample photodiode Part of the light is directed to the reference photodiode by the beam splitter to obtain a reference signal for compensation of intensity fluctuation of the light source A slit in front of the reference photodiode cuts out light of the sample bandwidth Wavelength selection is made by rotating the grating which is driven directly by a stepper motor This configuration allows fast change of the wavelength The cutoff filter is moved into the lightpath above 370 nm to reduce higher order light Lens Mirror M1 Sample diode Flow cell Grating Mirror M2 Beam splitter N Reference diode ba Figure 1 Optical Path of the Variable Wavelength Detector Agilent 1260 Infinity VWD User Manual 11 1 Introduction to the Variable Wavelength Detector Flow Cell A variety of flow cell cartridges can be inserted using the same quick and simple mounting system Table1 Flow Cell D Figure 2 Cartridge Type Flow Cell ata STD Semi micro High Pressure Micro Maximum pressure 40 4 40 4 400 40 40 4 bar MPa Path length
13. 1 Introduction to the Variable Wavelength Detector Introduction to the Detector 10 The Agilent 1260 Infinity variable wavelength detector is designed for highest optical performance GLP compliance and easy maintenance with data rate up to see Peakwidth Settings on page 66 13 Hz for standard HPLC with G1314B VWD VL 55 Hz for fast HPLC G1314C VWD VL deuterium lamp for highest intensity and lowest detection limit over a wavelength range of 190 to 600 nm e optional flow cell cartridges standard 10 mm 14 uL high pressure 10 mm 14 uL micro 5 mm 1 uL semi micro 6 mm 5 uL are available and can be used depending on the application needs easy front access to lamp and flow cell for fast replacement and built in holmium oxide filter for fast wavelength accuracy verification For specifications refer to Table 4 on page 27 Two version of the Agilent 1260 Infinity variable wavelength detector are available G1314B Agilent 1260 Infinity Variable Wavelength Detector VL G1314C Agilent 1260 Infinity Variable Wavelength Detector VL high data rates for fast HPLC Agilent 1260 Infinity VWD User Manual Introduction to the Variable Wavelength Detector 1 Optical System Overview The optical system of the detector is shown in the figure below Its radiation source is a deuterium arc discharge lamp for the ultraviolet UV wavelength range from 190 to 600 nm The light beam from the deuterium lamp passes
14. 10 conical 6 conical 10 conical 5 mm Volume 14 5 14 1 pL Inlet i d 0 17 0 17 0 17 0 1 mm Inlet length 750 750 750 555 mm Outlet i d 0 25 0 25 0 25 0 25 mm Outlet length 120 120 120 120 mm Materials in contact with SST quartz SST quartz SST quartz SST quartz solvent PEEK PTFE Kapton PTFE 12 Agilent 1260 Infinity VWD User Manual Introduction to the Variable Wavelength Detector 1 G1314B C Lamp The light source for the UV wavelength range is a deuterium lamp As a result of plasma discharge in a low pressure deuterium gas the lamp emits light over the 190 to 600 nm wavelength range Source Lens Assembly The source lens receives the light from the deuterium lamp and focuses it onto the entrance slit Entrance Slit Assembly The entrance slit assembly has an exchangeable slit The standard one has a 1 mm slit For replacement and calibration purposes to optimize the alignment a slit with a hole is needed Filter Assembly The filter assembly is electromechanically actuated During wavelength calibrations it moves into the light path The filter assembly has two filters installed and is processor controlled OPEN nothing in light path CUTOFF cut off filter in light path at A gt 370 nm HOLMIUM holmium oxide filter for wavelength check A photo sensor determines the correct position Agilent 1260 Infinity VWD User Manual 13 1 Introduction to the Variable Wavelength Detector Holmium oxide filt
15. 5 m CAN cable Agilent module to module 1 m Description Cross over network cable shielded 3 m for point to point connection Twisted pair network cable shielded 7 m for point to point connection Agilent 1260 Infinity VWD User Manual 155 11 Identifying Cables RS 232 Cable Kit p n Description G1530 60600 RS 232 cable 2 m RS232 61600 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 8m 156 Agilent 1260 Infinity VWD User Manual External Contact Cable ebe 6 o of 10 6 15 9 AL Identifying Cables One end of this cable provides a 15 pin plug to be connected to Agilent modules interface board The other end is for general purpose Agilent Module Interface Board to general purposes 11 p n G1103 61611 Color Pin Agilent Signal Name module White 1 EXT 1 a Brown 2 EXT 1 EE Green 3 EXT2 Yellow 4 EXT 2 Grey 5 EXT 3 Pink 6 EXT 3 Blue 7 EXT 4 Red 8 EXT 4 Black 9 Not connected Violet 10 Not connected Grey pink 11 Not connected Red blue 12 Not connected White green 13 Not connected Brown green 14 Not connected White yellow 15 Not connected Agilent 1260 Infinity VWD User Manual 157 11 Identifying Cables E
16. Agilent Liquid Chromatograph you can ensure optimum performance by installing the following configurations These configurations optimize the system flow path ensuring minimum delay volume One Stack Configuration Ensure optimum performance by installing the modules of the Agilent 1260 Infinity LC System in the following configuration See Figure 4 on page 35 and Figure 5 on page 36 This configuration optimizes the flow path for minimum delay volume and minimizes the bench space required Agilent 1260 Infinity VWD User Manual Solvent cabinet Vacuum degasser Local User Interface Autosampler Column compartment Detector Installing the Detector Optimizing the Stack Configuration Figure 4 Recommended Stack Configuration for 1260 Front View Agilent 1260 Infinity VWD User Manual 3 35 3 Installing the Detector Optimizing the Stack Configuration Remote cable CAN Bus cable to local user interface CAN Bus cable Analog detector signal 1 or 2 outputs per detector AC power LAN to LC ChemStation location depends on detector Figure 5 Recommended Stack Configuration for 1260 Rear View 36 Agilent 1260 Infinity VWD User Manual Installing the Detector 3 Two Stack Configuration To avoid excessive height of the stack when the autosampler thermostat is added to the system it is recommended to form two stacks Some users prefer the lower height
17. Hz x 5 6 220 VA 85 W 290 BTU Maximum 0 55 C 32 131 F 40 70 C 4 158 F lt 95 96 at 25 40 C 77 104 F Non condensing Up to 2000 m 6562 ft Up to 4600 m 15091 ft For storing the module Installation category II Pollution degree 2 For indoor use only Agilent 1260 Infinity VWD User Manual Performance Specifications Site Requirements and Specifications 2 Performance Specifications G1314B Table3 Performance Specifications G1314B Type Specification Comments Detection type Double beam photometer Light source Wavelength range Short term noise ASTM Drift Linearity Wavelength accuracy Maximum data rate Band width Flow cells Deuterium lamp 190 600 nm t 0 510 AU at 254 nm 3 10 AU h at 254 nm gt 2 AU 5 upper limit tinm 13Hz 6 5 nm typical Standard 14 pL volume 10 mm cell path length and 40 bar 580 psi pressure maximum High pressure 14 pL volume 10 mm cell path length and 400 bar 5800 psi pressure maximum Micro 1 uL volume 5 mm cell path length and 40 bar 580 psi pressure maximum Semi micro 5 uL volume 6 mm cell path length and 40 bar 580 psi pressure maximum See Specification Conditions on page 29 See Specification Conditions on page 29 See Specification Conditions on page 29 Self calibration with deuterium lines verification with holmium oxide filter Can be repaired on component
18. Kit BACK Gasket Kit FRONT and 4 mm hexagonal wrench Window screw kit includes 2 quartz windows 2 compression washers 2 window holders 2 window screws and 10 washers Agilent 1260 Infinity VWD User Manual 1 Window screw 1 2 Washers 2 3 Compression washer K P 4 4 Window holder 9 5 Quartz window 6 Gasket front 7 Gasket back Figure 43 Micro Flow Cell 3 mm 2 uL Agilent 1260 Infinity VWD User Manual Parts and Materials for Maintenance Micro Flow Cell 3 mm 2 pL 10 139 10 Parts and Materials for Maintenance Semi micro Flow Cell 6 mm 5 pL Item p n Description G1314 60083 Semi micro flow cell 6 mm 5 pL 40 bar 5021 1823 Capillary column detector SST 400 mm lg 0 12 mm i d 1 G1314 20047 Cell screw G1314 65056 Semi micro cell kit includes two quartz windows one gasket 1 one 2 and two PTFE gaskets 2 79853 29100 Conical spring kit 10 pk 3 79853 22500 4 Ring SST 2 pk 4 79853 68743 PTFE gasket round hole i d 2 5 mm o d 8 mm 10 pk 5 79853 68742 Window quartz kit 2 pk 6 Semi micro 1 gasket long hole 1 5 x 3 5 mm PTFE 7 Semi micro 2 gasket long hole 2 x 4 mm PTFE 1 Cell screw 2 Conical springs 3 Ring SST 4 PTFE gasket 5 Quartz window 6 Semi micro gasket 1 7 Semi micro gasket 2 Figure 44 Semi micro Flow Cell 6 mm 5 uL 140 Agilent 1260 Infinity VWD User Manual Parts and Materials for Maintenance 10 High Pressure Flow
19. Lamp turn on and off of UV lamp si Control Lamp Error Method 34 At Power On automatic lamp on at Fu Online Spectra um power on NU ULIS on Take current method Error Method take error method or Help i Cof current method in case of an error Analog Output Range Analog Output Range can be set to Coiv Ciy either 100 mV or 1 V full scale see Analog Output Settings on page 64 Lamp Type can be set to either r t Power On m Lamp Type G1314 60100 standard VWD lamp or Tur lamp on 6131 4 B0100 2140 0590 DAD lamps see also Exchanging a Lamp on page 119 Automatic Tum On Automatic Turn On lamps can be programmed detector must be on for Tum lamp on at this Date 9322005 lt ddimmppyy gt Help online help hhmmiss DK Cancel Help Figure 21 Detector control settings Time Agilent 1260 Infinity VWD User Manual 61 4 Using the Detector Online Spectra 1 To view the online spectra select Online Spectra This online spectrum is taken during a stop flow condition only while the peak is kept in the flow cell see Scanning with the VWD on page 63 Q Set up VWD Signal Hw scan y lo x of Control mAU fy Online Spectra 8 Not Ready Information 800 J Help i 800 400 200 lj r r r r r r f 200 225 250 275 300 325 350 375 nm 100 00 to 1000 0
20. Line driver RFI filter 250mA External 4x External contacts lt contact connector RH filter Agilent 1260 Infinity VWD User Manual 163 12 Hardware Information 164 There are general purpose cables available to connect the BCD output see BCD Cables on page 153 and the external outputs see External Contact Cable on page 157 to external devices Table 15 Detailed connector layout 1200 Pin Signal name BCD digit 1 BCD 5 20 2 BCD7 80 3 BCD 6 40 4 BCD4 10 5 BCD 0 1 6 BCD 3 8 7 BCD2 4 8 BCD 1 2 9 Digital ground 10 BCD 11 800 11 BCD 10 400 12 BCD 9 200 13 BCD 8 100 15 5V Low LAN Communication Interface Board The Agilent modules have one optional board slot that allows to add an interface board to the modules Some modules do not have this interface slot Refer to Interfaces on page 169 for details p n Description G1369B or G1369 60002 Interface board LAN G1369C or G1369 60012 Interface board LAN Agilent 1260 Infinity VWD User Manual Hardware Information 12 One board is required per Agilent 1260 Infinity instrument It is recommended to add the LAN board to the detector with highest data rate For the configuration of the G1369 LAN Communication Interface card refer to its documentation The following cards can be used with the Agilent 1260 Infinity modules Table 16 LAN Boards Type Vendor Supported networks Interface board LAN p n
21. Online Spectra on page 62 displays the result Sample Scan minus Blank Scan Agilent 1260 Infinity VWD User Manual 63 4 Using the Detector Special Settings of the Detector Analog Output Settings 1 To change the Output Range of the analog outputs select VWD Control 2 To change the offset and the attenuation select VWD Signal gt More WD Control System 2 Analog Output Range can be set to either 100 mV or 1 V full scale Zero Offset can be set to either 100 mV or 1 V full scale Attenuation Limits 0 98 to 4000 mAU at discrete values for either 100 mV or 1 V full scale Ie Cad mm yy lime chtemnmss gt Figure 23 Analog Output Settings VWD Signal System 2 fy On 5 Not Ready Information Figure 24 Analog Output Settings 3 Change the values if required 64 Agilent 1260 Infinity VWD User Manual Using the Detector 4 Special Setpoints fe Set up VWD Signal of Control Pa Online Spectra 1 To change the offset and the attenuation select VWD Signal gt More gt Special Setpoints VWD Special Setpoints System 2 x Margin for negative Absorbance Use this field to modify the detector s signal handling to increase the margin 8 Not Ready Information Help Figure 25 Margin for negative Absorbance kinu mAU for negative absorbance Use this option if for example your solvent gradient produces a decreasing baseline absorbanc
22. Setting up an Analysis 46 Special Settings of the Detector 61 5 How to optimize the detector 69 Optimizing the Detector Performance 70 Match the Flow Cell to the Column 71 Set the Detector Parameters 74 6 Troubleshooting and Diagnostics 75 Overview of the Detector s Indicators and Test Functions 76 Status Indicators 77 Available Tests versus Interfaces 79 Agilent Lab Advisor Software 80 Agilent 1260 Infinity VWD User Manual Contents 7 Error Information 81 8 What Are Error Messages 82 General Error Messages 83 Detector Error Messages 90 Test Functions 99 Intensity Test 100 Cell Test 102 Wavelength Verification Calibration 104 ASTM Drift and Noise Test 106 Quick Noise Test 107 Dark Current Test 108 Holmium Oxide Test 110 Maintenance 113 Introduction to Maintenance 114 Warnings and Cautions 115 Overview of Maintenance 117 Cleaning the Module 118 Exchanging a Lamp 119 Exchanging a Flow Cell 122 Repairing the Flow Cells 124 Using the Cuvette Holder 126 Correcting Leaks 128 Replacing Leak Handling System Parts 129 Replacing the Interface Board 130 Replacing the Module s Firmware 131 Agilent 1260 Infinity VWD User Manual Contents 10 Parts and Materials for Maintenance 133 Overview of Maintenance Parts 134 Standard Flow Cell 10 mm 14 uL 135 Micro Flow Cell 5 mm 1 uL only for support 136 Micro Flow Cell 3 mm 2gL 138 Semi micro Flow Cell 6mm b uL 140 High Pressure Flow Cell 10 m
23. asp 2 For loading the firmware into the module follow the instructions in the documentation Agilent 1260 Infinity VWD User Manual 131 9 Maintenance Module Specific Information Table 14 Module Specific Information G1314B C G1314B VWD G1314C VWD SL Initial firmware A 06 02 A 06 02 Compatibility with 1100 1200 yes all modules should have the firmware from the same set series modules Conversion to emulation of possible if required G1314A or G1314B 132 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual 10 Parts and Materials for Maintenance Overview of Maintenance Parts 134 Standard Flow Cell 10 mm 14 uL 135 Micro Flow Cell 5 mm 1 pL only for support 136 Micro Flow Cell 3 mm 2ygL 138 Semi micro Flow Cell 6 mm 5b pL 140 High Pressure Flow Cell 10 mm 14 pL 141 Cuvette Holder 142 Leak Parts 143 Kits 144 This chapter provides information on parts for maintenance n Agilent Technologies 133 10 Parts and Materials for Maintenance Overview of Maintenance Parts p n 5181 1516 5181 1519 G1351 68701 G1369C or G1369 60012 64208 67001 61314 60100 G1314 60086 G1314 60081 61314 60082 61314 60083 G1314 60200 5067 4691 Description CAN cable Agilent module to module 0 5 m CAN cable Agilent module to module 1 m Interface board BCD with external contacts and BCD outputs Interface board LAN Instant Pilot G4208A requires firmware B
24. 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 original feature set is available again All these specific informations are described in the documentation provided with the firmware update tools The firmware update tools firmware and documentation are available from the Agilent web http www chem agilent com EN US SUPPORT DOWNLOADS FIRMWARE Pages LC aspx Agilent 1260 Infinity VWD User Manual Hardware Information 12 Optional Interface Boards BCD External Contact Board The Agilent 1200 Infinity Series modules have one optional board slot that allows to add an interface board to the modules Some modules do not have this interface slot Refer to Interfaces on page 169 for details Optional Interface Boards p n Description G1351 68701 Interface board BCD with external contacts and BCD outputs 2110 0004 Fuse for BCD board 250 mA The BCD board provides a BCD output for the bottle number of the Agilent 1200 Series autosampler and four external contacts The external contact closure contacts are relay contacts The maximum settings are 30 V AC DC 250 mA fused Board identification 12 Processor BCD BCD interface register connector
25. can be placed instead of a flow cell in the variable wavelength detector Standard cuvettes with standards in it for example National Institute of Standards amp Technology NIST holmium oxide solution standard can be fixed in it This can be used for wavelength verifications LOG P E N AS Parts required p n Description 1 1314 60200 Cuvette Holder 1 Cuvette with the standard e g NIST certified holmium oxide sample 126 Agilent 1260 Infinity VWD User Manual Maintenance 9 1 Locate the cuvette holder on the desk 3 Insert the cuvette with the sample into the holder The clear side of the cuvette must be visible Light path Clear side 2 Unscrew the bracket M 4 Replace the bracket and fix the cuvette Next Steps 5 Install the cuvette holder in the instrument correct position of the cuvette holder 6 Perform your Wavelength Verification Calibration see Wavelength Verification Calibration on page 104 to check the Agilent 1260 Infinity VWD User Manual 127 9 Maintenance Correcting Leaks Correcting Leaks When If a leakage has occurred in the flow cell area or at the capillary connections Tools required Description Tissue Wrench 1 4 inch 1 Remove the front cover 2 Use tissue to dry the leak sensor area 3 Observe the capillary connections and the flow cell area for leaks and correct if required 4 Replace the front cover
26. following information CCYWWSSSSS CC YWW SSSSS Agilent 1260 Infinity VWD User Manual Format country of manufacturing DE Germany e JP Japan CN China year and week of last major manufacturing change e g 820 could be week 20 of 1998 or 2008 real serial number 167 12 Hardware Information Electrical Connections Rear view of the module Security lever Slot for interface board Analog signals APG remote RS 232C CAN Configuration switch Power Figure 49 Rear view of detector NOTE The GPIB interface has been removed with the introduction of the 1260 Infinity modules 168 Agilent 1260 Infinity VWD User Manual Hardware Information 12 Interfaces The Agilent 1200 Infinity Series modules provide the following interfaces Table 17 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD LAN RS 232 Analog APG Special optional on board Remote Pumps G1310B Iso Pump 2 Yes No Yes 1 Yes G1311B Quat Pump G1311C Quat Pump VL G1312B Bin Pump G1312C Bin Pump VL 1376A Cap Pump G2226A Nano Pump G5611A Bio inert Quat Pump G4220A B Bin Pump 2 No Yes Yes No Yes G1361A Prep Pump 2 Yes No Yes No Yes CAN DC OUT for CAN slaves Samplers G1329B ALS 2 Yes No Yes No Yes THERMOSTAT for G1330B G2260A Prep ALS G1364B FC PS 2 Yes No Yes No Yes THERMOSTAT for G1330B G1364C FC AS CAN DC OUT for CAN slaves G1364D FC uS G1367E HiP ALS G1377A HiP micro ALS G2258A DL ALS
27. is advised to use the equipment in a manner as specified in this manual Safety Standards This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Operation 180 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 protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired Agilent 1260 Infinity VWD User Manual Appendix 13 the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses and the short circuiting of fuse holders must be avoided Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument
28. level Agilent 1260 Infinity VWD User Manual 25 2 Site Requirements and Specifications Table 3 Performance Specifications G1314B Type Specification Comments Control and data evaluation Analog outputs Communications Safety and maintenance GLP features Housing Agilent ChemStation for LC Recorder integrator 100 mV or 1 V output range 0 001 to 2 AU one output Controller area network CAN RS 232C APG Remote ready start stop and shut down signals LAN optional Extensive diagnostics error detection and display through Agilent ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas Early maintenance feedback EMF for continuous tracking of instrument usage in terms of lamp burn time with user settable limits and feedback messages Electronic records of maintenance and errors Verification of wavelength accuracy with built in holmium oxide filter All materials recyclable 26 Agilent 1260 Infinity VWD User Manual Site Requirements and Specifications 2 Performance Specifications G1314C Table4 Performance Specifications G1314C Type Specification Comments Detection type Double beam photometer Light source Wavelength range Short term noise ASTM Drift Linearity Wavelength accuracy Maximum data rate Band width Flow cells Control and data evaluation De
29. lines before opening any fittings 118 Agilent 1260 Infinity VWD User Manual Maintenance 9 Exchanging a Lamp When Tools required Parts required Preparations If noise or drift exceeds application limits or lamp does not ignite Description Screwdriver Pozidriv 1 PT3 p n Description G1314 60100 Deuterium lamp Turn the lamp OFF Injury by touching hot lamp If the detector has been in use the lamp may be hot gt If so wait for lamp to cool down If you want to use the Agilent DAD lamp instead of the VWD lamp you have to change the lamp settings in the VWD Configuration to lamp type 2140 0590 This ensures that the DAD lamp s filament heating is operated like in the DAD The specification are based on Deuterium lamp p n G1314 60100 and may be not achieved when other lamp types or aged lamps are used Agilent 1260 Infinity VWD User Manual 119 9 Maintenance Exchanging a Lamp 1 Press the release buttons and remove the front coverto 2 Unscrew the lamp cover and remove it have access to the lamp area 3 Unscrew disconnect and replace the lamp Insert fix and 4 Replace the lamp cover reconnect the lamp 120 Agilent 1260 Infinity VWD User Manual Maintenance 9 Excha ging Lamp 5 Replace the front cover Next Steps f 6 Reset the lamp counter as described in the User Interface documentation a Wj 7 Turn the lamp ON
30. of this arrangement even without the autosampler thermostat A slightly longer capillary is required between the pump and autosampler See Figure 6 on page 37 and Figure 7 on page 38 Instant Pilot Detector Column compartment Autosampler Fu ENX c S 7 E dy T 2 i Sais Thermostat for the ALS optional Solvent cabinet Degasser optional Pump Figure 6 Recommended Two Stack Configuration for 1260 Front View Agilent 1260 Infinity VWD User Manual 37 3 Installing the Detector Optimizing the Stack Configuration LAN to control software CAN Bus cable to Instant Pilot Thermo cable optional ee Remote cable 666666 AC Power CAN Bus cable AC Power Figure 7 Recommended Two Stack
31. on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current falls outside the lower limit the error message is generated Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board representative 2 Defective leak sensor Please contact your Agilent service representative 3 Leak sensor incorrectly routed being Please contact your Agilent service pinched by a metal component representative Agilent 1260 Infinity VWD User Manual Error Information 7 Leak Sensor Short Error ID 0082 The leak sensor in the module has failed short circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent 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 Defective leak sensor Please contact your Agilent service representative 2 Leak sensor incorrectly routed being Please contact your Agilent service pinched by a metal component representative Compensation Sensor Open Error ID 0081 The ambient compensation sensor NTC on the main board in the module has failed open circuit The resistance across the temperature compensation sensor NTC on the main board is dependent on ambient temperature
32. or module specific functions like internal events such as lamp control filter movements raw data collection and conversion to absorbance Firmware Updates Firmware updates can be done using your user interface PCand Firmware Update Tool with local files on the hard disk Agilent 1260 Infinity VWD User Manual Hardware Information 12 Instant Pilot G4208A with files from a USB Flash Disk Agilent Lab Advisor software B 01 03 and above The file naming conventions are PPPP_RVVV_XXX dlb where PPPP is the product number for example 1315AB 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 Update of main system can be done in the resident system only Update of the resident system can be done in the main system only Main and resident firmware must be from the same set Main FW update Resident System Main System Resident FW Update Figure 48 Firmware Update Mechanism Agilent 1260 Infinity VWD User Manual 161 12 Hardware Information 162 Some modules are limited in downgrading due to their main board version or their initial firmware revision For example a G1315C DAD SL cannot be downgraded
33. or service personnel is limited to the following TLVs Threshold Limit Values according to the American Conference of Governmental Industrial Hygienists Table 28 UV Radiation Limits Exposure day Effective Irradiance 8 hours 0 1 uW cm 10 minutes 5 0 uW cm Typically the radiation values are much smaller than these limits Table 29 UV Radiation Typical Values Position Effective Irradiance Lamp installed 50 cm distance average 0 016 W cm Lamp installed 50 cm distance maximum 0 14 uW cm Agilent 1260 Infinity VWD User Manual Appendix 13 Solvent Information Observe the following recommendations on the use of solvents Flow Cell Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical properties of the flow cell Prevent any crystallization of buffer solutions This will lead into a blokkage damage of the flow cell If the flow cell is transported while temperatures are below 5 degree C it must be assured that the cell is filled with alcohol Aqueous solvents in the flow cell can built up algae Therefore do not leave aqueous solvents sitting in the flow cell Add small of organic solvents e g Acetonitrile or Methanol 5 Solvents Brown glass ware can avoid growth of algae Always filter solvents small particles can permanently block the capillaries Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their
34. 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 module Use the status display of your user interface for finding the root cause module of the error A yellow blinking indicator indicates that the module is in resident mode e g during update of main firmware A fast yellow blinking indicator indicates that the module is in boot loader mode e g during update of main firmware In such as case try to re boot the module or try a cold start 78 Agilent 1260 Infinity VWD User Manual Troubleshooting and Diagnostics 6 Available Tests versus Interfaces Depending on the used interface the available tests and the screens reports may vary Preferred tool should be the Agilent Diagnostic Software see Agilent Lab Advisor Software on page 80 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 12 Available Tests versus Interface Interface Test Lab Advisor ChemStation Instant Pilot G4208A Wavelength Verification Re calibration Calibration Tests Maintenance Lamp Intensity Test Tests Tests Diagnosis ASTM Drift and Noise Test Tests n a n a Quick Noise Test T
35. respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like nitric acid sulfuric acid 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 2CHCl Oz gt 2COCl 2HCI This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol Agilent 1260 Infinity VWD User Manual 187 13 Appendix Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solutions of organic acids acetic acid formic acid and so on in organic solvents For example a 1 solution of acetic acid in methanol will attack steel Solutions containing strong complexing agents for example EDTA ethylene diamine tetra acetic acid Mixtures of carbon tetrachloride with 2 propanol or THF 188 Agilent 1260 Infinity VWD User Manual Appendix 13 Declaration of Conformity for HOX2 Filter Declaration of Conformity for HOX2 Filter We herewith inform you that the used in Agilents absorbance detectors listed in the table below meets the requirements of Nationa
36. stop run abort or finish and stop injection Receiver is any module performing run time controlled activities 9 START REQUEST L Request to start injection cycle for example by start key on any module Receiver is the autosampler Special Interfaces Some modules have module specific interfaces connectors They are described in the module documentation 174 Agilent 1260 Infinity VWD User Manual Hardware Information 12 Setting the 8 bit Configuration Switch without On board LAN The 8 bit configuration switch is located at the rear of the module This module does not have its own on board LAN interface It can be controlled through the LAN interface of another module and a CAN connection to that module Figure 51 Configuration switch settings depend on configured mode All modules without on board LAN e default should be ALL DIPS DOWN best settings Bootp mode for LAN and 19200 baud 8 data bit 1 stop bit with no parity for RS 232 DIP 1 DOWN and DIP 2 UP allows special RS 232 settings for boot test modes DIPS 1 2 must be UP plus required mode For normal operation use the default best settings Switch settings provide configuration parameters for serial communication protocol and instrument specific initialization procedures With the introduction of the Agilent 1260 Infinity all GPIB interfaces have been removed The preferred communication is LAN Agilent 1260 Infinity VWD User Manual 17
37. take note of the values displayed by lamp counters Enter these values or values slightly less than the displayed values as EMF limits and then reset the EMF counters to zero The next time the EMF counters exceed the new EMF limits the EMF flag will be displayed providing a reminder that maintenance needs to be scheduled This function is only available via LMD or Instant Pilot Agilent 1260 Infinity VWD User Manual 17 1 Introduction to the Variable Wavelength Detector Instrument Layout The industrial design of the module incorporates several innovative features It uses Agilent s E PAC concept for the packaging of electronics and mechanical assemblies This concept is based upon the use of expanded polypropylene EPP layers of foam plastic spacers in which the mechanical and electronic boards components of the module are placed This pack 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 plastic layers help cushion the electronic and mechanical parts from physical shock and the metal inner cabinet shields the internal electronics from electromagnetic interference and als
38. the detector is missing During lamp ignition the processor monitors the heater current If the current does not rise above the lower limit within 1 the error message is generated Probable cause Suggested actions 1 Lamp disconnected Ensure the lamp is connected 2 Ignition started without the top foam in Please contact your Agilent service place representative 3 Defective main board Please contact your Agilent service representative 4 Defective or non Agilent lamp Exchange the lamp 5 Defective power supply Please contact your Agilent service representative Agilent 1260 Infinity VWD User Manual Wavelength calibration setting failed Error ID 7310 Error Information 7 The intensity maximum was not found during wavelength calibration Calibration 0 Failed Calibration 1 Failed Probable cause 1 Lamp is OFF 2 Incorrect flow cell installation 3 Flow cell contamination or air bubbles 4 Intensity too low 5 Current step value too far from maximum 6 Misaligned defective grating assembly 7 Defective main board Agilent 1260 Infinity VWD User Manual Zero order calibration failed 656 nm calibration failed Suggested actions Switch on the lamp Ensure the flow cell are installed correctly Clean replace flow cell windows or remove air bubbles Replace lamp Repeatthe calibration Please contact your Agilent service representative Please contact your Agilent service represen
39. the integrator side Otherwise the integrator prints START not ready Agilent 1260 Infinity VWD User Manual Identifying Cables 11 Agilent Module to 3396 Series III 3395B Integrators p n 03396 61010 Pin 33XX Pin Agilent Signal Name Active module TTL 9 1 White Digital ground NC 2 Brown Prepare run Low 80 3 3 Gray Start Low x NC 4 Blue Shut down Low o e e NC 5 Pink Not connected le NC 6 Yellow Power on High p 14 7 Red Ready High 4 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent Module to Agilent 35900 A D Converters p n 5061 3378 Pin 35900 A D Pin Agilent Signal Name Active module 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 Yellow 6 Yellow Power on High 7 Red 7 Red Ready High 8 Green 8 Green Stop Low 9 Black 9 Black Start request Low Agilent 1260 Infinity VWD User Manual 151 11 152 Identifying Cables Agilent Module to General Purpose p n 01046 60201 Wire Color Pin Agilent Signal Name Active module TTL White 1 Digital ground A Q 1 Dn Brown 2 Prepare run Low 00 em OB KEY Gray 3 Start Low oo poe uH S EE te 4 Shut down Low og Pink 5 Not connected oo BB Yellow 6 Power on Hi
40. the path length from 6 mm to 10 mm When increasing the path length the cell volume usually increases in the example from 5 14 uL Typically this causes more peak dispersion As demonstrated this did not affect the resolution in the gradient separation in the example shown below As a rule of thumb the flow cell volume should be about 1 3 of the peak volume at half height To determine the volume of your peaks take the peak width as reported in the integration results multiply it by the flow rate and divide it by 3 Agilent 1260 Infinity VWD User Manual How to optimize the detector 5 Analysis of pesticide standard 6 mm optical path length Absorbance T0 mm optical path length i MET Nila tify N p ll i 1 i Vi J n J m na AN ud e gd ME NW MTMM 1g 20 30 Time min Figure 28 Influence of Cell Path Length on Signal Height Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards To check photometric accuracy of the Agilent 1200 Series Infinity Variable Wavelength Detector it is necessary to have more precise information on path lengths of the VWD flow cells The correct response is expected response correction factor Please find below the details of the Agilent 1200 Infinity Series Variable Wavelength Detector flow cells Table 11 Correction factors for Agilent VWD flow cel
41. 0 Peak Width Response Time Data Rate G1314C VWD SL Peak Width min Response Time s Data Rate Hz 0 00125 0 031 55 gt 0 00125 0 031 27 5 gt 0 0025 0 062 13 74 gt 0 005 0 12 13 74 20 01 0 25 13 74 20 025 0 5 13 74 20 05 1 0 6 87 20 10 2 0 3 43 20 20 4 0 172 20 40 8 0 0 86 Values in the User Interface may be rounded Agilent 1260 Infinity VWD User Manual 67 4 Using the Detector Special Settings of the Detector 68 Agilent 1260 Infinity VWD User Manual s Agilent 1260 Infinity VWD User Manual ee 5 How to optimize the detector o o E e e a e d Optimizing the Detector Performance 70 e Match the Flow Cell to the Column 71 Set the Detector Parameters 74 This chapter gives hints on how to select the detector parameters and the flow cell XE Agilent Technologies 69 5 How to optimize the detector Optimizing the Detector Performance The detector has a variety of parameters that can be used to optimize 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 a rule of thumb for optimizing the detector parameters 70 Agilent 1260 Infinity VWD User Manual How to optimize the detector 5 olumn Match the Flow Cell to t Match the Flow Cell to the Column Figure 27 on page 71 recommends the flow cell that matches the column used If more than one selection is appropriate use
42. 02 08 or above Deuterium lamp Standard flow cell 10 mm 14 pL 40 bar Micro flow cell 5 mm 1 uL 40 bar High pressure flow cell 10 mm 14 pL 400 bar Semi micro flow cell 6 mm 5 pL 40 bar Cuvette Holder Front Cover Leak handling parts For leak handling parts see Leak Parts on page 143 134 Agilent 1260 Infinity VWD User Manual Parts and Materials for Maintenance 10 Standard Flow Cell 10 mm 14 pL 1 Cell screw 2 Conical springs 3 Ring 2 IN 4 Gasket 2 IN 5 Quartz window 6 Gasket 1 OUT 7 Ring 1 OUT Item p n G1314 60086 5062 8522 G1314 65061 G1314 65062 79853 29100 G1314 65066 G1314 65064 79853 68742 G1314 65063 G1314 65065 c Oi A C N Description Standard flow cell 10 mm 14 pL 40 bar Capillary column detector PEEK 600 mm lg 0 17 mm i d 1 16 inch o d Cell Repair Kit includes 2x Gasket 1 2x Gasket 2 2x Window Quartz Cell screw kit Conical spring kit 10 pk Ring 2 kit IN small hole i d 1 mm PEEK 2 pk Gaskets 2 IN small hole i d 1 mm KAPTON 10 pk Window quartz kit 2 pk Gasket 1 kit OUT large hole i d 2 4 mm KAPTON 2 pk Ring 1 kit OUT large hole i d 2 4 mm PEEK 2 pk Figure 41 Standard Flow Cell 10 mm 14 uL Agilent 1260 Infinity VWD User Manual 135 10 Parts and Materials for Maintenance Micro Flow Cell 5 mm 1 pL only for support Item p n Description G1314 60081 Micro flow cell 5 mm 1 uL 40 bar 5021 18
43. 110261 Status Passed Start Time 6 9 2010 12 40 40 PM Stop Time 6 9 2010 12 45 46 PM Test Procedure Result Value W 1 Check Prerequisites Accumulated UY Lamp Burn Time 178 61h V 2 Measure Noise UV Lamp On Time 228h YW 3 Evaluate Data Signal Noise value at 254 nm UV 0 006 mAU Absorbance mAU 1 2354 1 238 1 24 1 242 1 244 1 2453 J r 0 0 5 25 Time min Figure 35 Quick Noise Test Agilent Lab Advisor Agilent 1260 Infinity VWD User Manual 107 8 Test Functions Dark Current Test The dark current test measures the leakage current from the sample and reference circuits The test is used to check for defective sample or reference diodes or ADC circuits which may cause non linearity or excessive baseline noise During the test the lamp is switched off Next the leakage current from both diodes is measured Dark Current Test Failed Probable cause Suggested actions 1 Defective sample or reference diode Please contact your Agilent service representative 2 Defective sample or reference ADC board Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative 108 Agilent 1260 Infinity VWD User Manual Test Functions 8 Dark Current Test Test Name Dark Current Test Description The test measures the dark current from the detector optic Module G1314CJP32110261 Status Passed Start
44. 23 Capillary column detector SST 400 mm lg 0 12 mm i d 1 G1314 20047 Cell screw G1314 65052 Cell kit micro comprises two windows two gaskets 1 and two gaskets 2 2 79853 29100 Conical spring kit 10 pk 3 79853 22500 Ring SST 2 pk 5 79853 68742 Window quartz kit 2 pk 4 79853 68743 PTFE gasket round hole i d 2 5 mm o d 8 mm 10 pk 6 G1314 65053 Gasket 2 PTFE quantity 10 136 Agilent 1260 Infinity VWD User Manual Parts and Materials for Maintenance 10 Micro Flow Cell 5 mm 1 pL only for support Cell screw Conical springs Ring SST Gasket 1 Window quartz Gasket 2 oo F c N gt 1 i i Figure 42 Micro Flow Cell b mm 1 uL 40 bar Agilent 1260 Infinity VWD User Manual 137 10 Parts and Materials for Maintenance Micro Flow Cell 3 mm 2 pL Item p n G1314 60087 5021 1823 79883 22402 2 5062 8553 3 79883 28801 4 79883 22301 5 1000 0488 6 G1315 68710 7 79883 68702 G1314 87301 G1314 87302 G1315 68713 79883 68703 138 Description Micro flow cell without I D tag 3 mm 2 pL 120 bar Capillary column detector SST 400 mm lg 0 12 mm i d Window screw Washer kit 10 pk Compression washer Window holder Quartz window Gasket FRONT PTFE 1 3 mm hole inlet side 12 pk Gasket BACK PTFE 1 8 mm hole outlet side 12 pk Capillary IN 0 12 mm 310 mm Ig Capillary OUT 0 17 mm 120 mm lg Cell repair kit semi micro includes window screw kit Gasket
45. 314C on page 27 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 C h 1 8 F h Turbulences around one minute or less can be ignored Condensation within the module Condensation will damage the system electronics Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation This module is designed to operate in a typical electromagnetic environment i e where RF transmitters such as mobile telephones may not be used in close proximity Agilent 1260 Infinity VWD User Manual 23 2 Site Requirements and Specifications Physical Specifications 24 Table2 Physical Specifications Type Specification Comments Weight 11 kg 25 Ibs Dimensions 140 x 345 x 435 mm 5 5 x 13 5 x 17 inches height x width x depth Line voltage Line frequency Power consumption Ambient operating temperature Ambient non operating temperature Humidity Operating altitude Non operating altitude Safety standards IEC CSA UL 100 240 VAC 10 Wide ranging capability 50 or 60
46. 5 12 Hardware Information 176 The following tables represent the configuration switch settings for the modules without on board LAN only Table 20 8 bit Configuration Switch without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baudrate Data Parity Bits Reserved 1 0 Reserved TEST BOOT 1 1 RSVD SYS RSVD RSVD FC The LAN settings are done on the LAN Interface Card G1369B C Refer to the documentation provided with the card Communication Settings for RS 232C The communication protocol used in the column compartment supports only hardware handshake CTS RTR Switches 1 in down and 2 in up position define that the RS 232C parameters will be changed Once the change has been completed the column instrument must be powered up again in order to store the values in the non volatile memory Table21 Communication Settings for RS 232C Communication without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS232C 0 1 Baudrate Data Bits Parity Use the following tables for selecting the setting which you want to use for RS 232C communication The number 0 means that the switch is down and 1 means that the switch is up Agilent 1260 Infinity VWD User Manual Hardware Information 12 Table 22 Baudrate Settings without on board LAN Switches Baud Rate Switches Baud Rate 3 4 3 4 5 0 0 9600 1 0 0 9600 0 0 1200 1 0 1 14400 0 1 2400 1 1 0 19200 0 1 4800 1 1 1 38400
47. 8 Give the lamp more than 10 min to warm up Perform Wavelength Verification Calibration on page 104 to check the correct positioning of the lamp Agilent 1260 Infinity VWD User Manual 121 9 Maintenance Exchanging a Flow Cell When Tools required Parts required OR OR OR Preparations If an application needs a different type of flow cell or the flow cell needs repair Description Wrench 1 4 inch 1 1 1 1 Turn the lamp OFF p n G1314 60086 G1314 60081 G1314 60083 G1314 60082 Description Standard flow cell 10 mm 14 pL 40 bar Micro flow cell 5 mm 1 uL 40 bar Semi micro flow cell 6 mm 5 pL 40 bar High pressure flow cell 10 mm 14 pL 400 bar 1 Press the release buttons and remove the front coverto 2 Disconnect the inlet and outlet capillaries have access to the lamp area 122 Agilent 1260 Infinity VWD User Manual Maintenance 9 3 Unscrew the thumb screws parallel and remove the flow cell If you want to maintain flow cell parts see Repairing the Flow Cells on page 124or the information provided with your flow cell 4 Press the flow cell completely into the slot and tighten the cell screws both parallel until the mechanical stop Reconnect the inlet and outlet capillaries to the flow cell 7J 5 Replace the front cover Next Steps 6 To check for leaks establish a flow and observe the
48. AM m Test Procedure W 1 Check Prerequisites v 2 Perform Intensity Test UV Lamp On Time Ji3tho VY 3 Evalate Data 1028 Cari SUBIT Cors ZMT Cons Intensity Counts 2 3309E 05 2E 05 1 5E 05 1E 05 50000 1028 471 1 190 500 800 Wavelength nm Figure 30 Intensity Test with Agilent Lab Advisor Intensity Test Failed Probable cause Suggested actions 1 Empty flow cell Ensure the flow cell is filled with water 2 Flow cell windows dirty Repeat the test with the flow cell removed If the test passes exchange the flow cell windows 3 Optics defect Please contact your Agilent service representative 4 Defective lamp or optics Exchange the lamp Agilent 1260 Infinity VWD User Manual 101 8 Test Functions Cell Test 102 The cell test compares the intensity of the deuterium lamp measured by the sample and reference diodes unfiltered and not logarithmized when the grating is in the zero order position The resulting intensity ratio sample reference is a measure of the amount of light absorbed by the flow cell The test can be used to check for dirty or contaminated flow cell windows When the test is started the gain is set to 1 To eliminate effects due to absorbing solvents the test should be done with water in the flow cell Limits No real limit The reason is that it depends on the position alignment of the reference side beam splitter referen
49. Agilent Technologies Fast Ethernet Ethernet 802 3 G1369B or G1369 60002 or RJ 45 10 100Base TX Interface board LAN p n recommended for re ordering G1369C or G1369 60012 LAN Communication Interface Agilent Technologies Fast Ethernet Ethernet 802 3 board p n G1369A or RJ 45 10 100Base TX G1369 60001 obsolete J4106A Hewlett Packard Ethernet 802 3 RJ 45 10Base T J4105A Hewlett Packard Token Ring 802 5 DB9 RJ 45 10Base T J4100A Hewlett Packard Fast Ethernet Ethernet 802 3 RJ 45 10 100Base TX BNC 10Base2 1 These cards may be no longer orderable Minimum firmware of these Hewlett Packard JetDirect cards is A 05 05 Recommended LAN Cables 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 Agilent 1260 Infinity VWD User Manual 165 12 Hardware Information Electrical Connections The CAN bus is a serial bus with high speed data transfer The two connectors for the CAN bus are used for internal module data transfer and synchronization One analog output provides signals for integrators or data handling systems The interface board slot is used for external contacts and BCD bottle number output or LAN connections The REMOTE connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features such as
50. Cell 10 mm 14 pL Item p n 1 Cell screw 2 Ring PEEK 3 Quartz window 4 Gasket KAPTON Figure 45 G1314 60082 G1315 87311 G1314 20047 61314 65054 Agilent 1260 Infinity VWD User Manual Description High pressure flow cell 10 mm 14 pL 400 bar Capillary column detector 380 mm lg 0 17 i d includes ferrule front 1 16 ferrule back 1 16 and fitting 1 16 Cell screw Cell kit Agilent comprises two windows two KAPTON gaskets and two PEEK rings Ring PEEK kit Window quartz kit Gasket kit KAPTON High Pressure Flow Cell 10 mm 14 pL 141 10 Parts and Materials for Maintenance Cuvette Holder For information the use of the cuvette holder refer to Using the Cuvette Holder on page 126 p n Description G1314 60200 Cuvette Holder Figure 46 Cuvette Holder 142 Agilent 1260 Infinity VWD User Manual Leak Parts Item p n 3 5041 8388 4 5041 8389 5 5041 8387 6 5062 2463 7 5062 2463 Parts and Materials for Maintenance 10 Leak Parts Description Leak funnel Leak funnel holder Tube clip Corrugated tubing PP 6 5 mm id 5m Corrugated tubing PP 6 5 mm id 5m Figure 47 Leak Parts Agilent 1260 Infinity VWD User Manual 143 10 Parts and Materials for Maintenance Kits HPLC System Tool Kit HPLC System Tool Kit p n G4203 68708 contains some accessories and tools needed for installation and maintenance of the module Accessory Kit Acce
51. Configuration for 1260 Rear View 38 Agilent 1260 Infinity VWD User Manual Installing the Detector 3 Installing the Detector Parts required Preparations p n Description Detector Power cord Agilent ChemStation or other control software 1 1 1 LAN cable cross over or twisted pair network cable 1 1 G4208A Instant Pilot For other cables see below and section Cable Overview on page 146 Instant Pilot G4208A is optional Other LC modules must have appropriate firmware installed to work with the detector Locate bench space Provide power connections Unpack the detector Before adding the detector into an existing system assure that the existing modules have been updated to firmware revision that is supported by the control software 1 Install the LAN interface board in the detector if required see Replacing the Interface Board on page 130 2 Place the detector in the stack or on the bench in a horizontal position Agilent 1260 Infinity VWD User Manual 39 3 Installing the Detector 3 Ensure the line power switch at the front of the detector is OFF Status indicator green yellow red fF _J ii d eF Line power switch with green light Figure 8 Front View of Detector The figure above shows the flow cell already installed The flow cell area is closed with a cover The flow cell has to be installed as described in Flow Connectio
52. 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 Defective main board Please contact your Agilent service representative Agilent 1260 Infinity VWD User Manual 87 7 88 Error Information Compensation Sensor Short Error ID 0080 The ambient compensation sensor NTC on the main board in the module has failed short 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 falls below the lower limit the error message is generated Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative Fan Failed Error ID 0068 The cooling 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 not overheat inside Agilent 1260 Infinity VWD User M
53. Time 5 2 2010 4 03 32 PM Stop Time 5 2 2010 4 07 41 PM r Test Procedure Result v 1 Check Prerequisites Maximum Sample Intensity Measured 4 064 Counts W 2 Perform Dark Current Test Maximum Reference Intensity Measured 4 020 Counts v 3 Switch UV Lamp on again v 4 Evaluate Data Intensity Counts 4064 4060 4050 4040 1 D 1 1 1 1 1 D 1 1 0 2 0 4 0 6 0 8 1 1 2 1 4 1 6 1 8 1 9947 Time min Intensity Counts 4020 4010 4000 3996 1 D 1 1 1 D 1 D 1 1 0 2 0 4 0 6 0 8 il 1 2 1 4 1 6 1 8 1 9947 Time min Figure 36 Dark Current Test Agilent Lab Advisor Agilent 1260 Infinity VWD User Manual 109 Test Functions Holmium Oxide Test 110 This test verifies the calibration of the detector against the three wavelength maxima of the built in holmium oxide filter The test displays the difference between the expected and measured maxima The figure below shows a holmium test spectrum The Holmium Oxide Test is available in Agilent Lab Advisor preferred tool Agilent Instant Pilot G4208A via More Diagnosis VWD Holmium Spectrum Test The test uses the following holmium maxima 360 8 nm 418 5 nm 536 4 nm See also Declaration of Conformity for HOX2 Filter on page 189 When to do the Test after recalibration as part of the Operational Qualification Performance Verification procedure or after flow cell maintenance o
54. al Hardware Information 12 Interfaces Overview CAN The CAN is inter module communication interface It is a 2 wire serial bus system supporting high speed data communication and real time requirement LAN The modules have either an interface slot for an LAN card e g Agilent G1369B C LAN Interface or they have an on board LAN interface e g detectors G1315C D DAD and G1365C D MWD This interface allows the control of the module system via a PC with the appropriate control software If an Agilent detector DAD MWD FLD VWD RID is in the system the LAN should be connected to the DAD MWD FLD VWD RID due to higher data load If no Agilent detector is part of the system the LAN interface should be installed in the pump or autosampler 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 There is no configuration possible on main boards with on board LAN These are pre configured for 19200 baud 8 data bit with no parity and one start bit and one stop bit are always used not selectable The RS 232C is designed as DCE data communication equipment with a 9 pin male SUB D type connector The pins are defined as Agilent 1260 Infinity VWD User Manual 171 12 Hardware Information 172
55. al setpoints 65 special settings 61 stop flow condition 62 the detector 45 the cuvette holder 126 turnon 52 typical chromatogram 50 UV radiation 186 V voltage range 24 wW warnings and cautions 115 wavelength accuracy 25 27 calibration 104 range 190 600 nm 25 27 recalibration 76 weight 24 Agilent 1260 Infinity VWD User Manual Index Agilent 1260 Infinity VWD User Manual 195 www agilent com In This Book This manual covers the Agilent 1260 Infinity Variable Wavelength Detector G1314B C The manual describes the following introcduction and specifications installation using and optimizing troubleshooting and diagnose maintenance parts identification hardware information safety and related information Agilent Technologies 2011 2012 Printed in Germany 05 2012 G1314 90013 Rev B RES Agilent Technologies
56. andard flow cell installed Degasser optional Column Compartment optional Agilent ChemStation or Instant Pilot G4208 optional for basic operation System should be correctly set up for LAN communication with the Agilent ChemStation Zorbax Eclipse XDB C18 4 6 x 150 mm 5 um p n 993967 902 or an equivalent column Agilent isocratic checkout sample p n 01080 68704 Agilent 1260 Infinity VWD User Manual Using the Detector 4 Conditions A single injection of the isocratic test standard is made under the conditions given in Table 8 on page 49 Table8 Conditions Flow 1 5 mL min Stoptime 8 min Solvent 100 30 water 70 Acetonitrile Temperature Ambient Wavelength sample 254 nm Injection Volume Tul Column Temperature optional 25 C or ambient Agilent 1260 Infinity VWD User Manual 49 4 Using the Detector Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 10 on page 50 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 DAD1 A Sig 254 4 Ref 500 100 04101410 140003 D mAU yt a e e La a a CC CS CO 0T min Figure 10 Typical Chromatogram with UV detector Optimization of the System The settings used for this analysis are speci
57. anual Probable cause 1 Fan cable disconnected 2 Defective fan 3 Defective main board Open Cover Error ID 0205 The top foam has been removed Error Information 7 Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative The sensor on the main board detects when the top foam is in place If the foam is removed during operation the lamp and grating drive power is switched off and the error message is generated Probable cause 1 The top foam was removed during operation 2 Foam not activating the sensor 3 Dirty or defective sensor Agilent 1260 Infinity VWD User Manual Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative 89 7 Error Information Detector Error Messages 90 These errors are detector specific UV lamp no current Error ID 7450 The lamp anode current is missing The processor continually monitors the anode current drawn 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 Lamp disconnected Ensure the lamp connector is seated firmly 2 Top foam removed while lamp is on Please contact your Agilent service representative
58. blems 76 Agilent 1260 Infinity VWD User Manual Troubleshooting and Diagnostics 6 Status Indicators Status Indicators Two status indicators are located on the front of the detector The lower left indicates the power supply status the upper right indicates the detector status Status indicator green yellow red Line power switch with green light Figure 29 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 Agilent 1260 Infinity VWD User Manual 71 6 Troubleshooting and Diagnostics Module Status Indicator The module status indicator indicates one of six possible module conditions When the status indicator is OFF and power switch light is on the module is in a prerun condition and is ready to begin an analysis A green status indicator indicates the module is performing an analysis run mode A yellow indicator indicates a not ready condition The module is in a not ready state when it is waiting for a specific condition to be reached or completed for example immediately after changing a set point or while a self test procedure is running An error condition is indicated when the status 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
59. built in test functions RE Agilent Technologies 99 Test Functions Intensity Test 100 The intensity test measures the intensity of the deuterium lamp over the full VWD wavelength range 190 600 nm The test can be used to determine the performance of the lamp and to check for dirty or contaminated flow cell windows When the test is started the gain is set to zero To eliminate effects due to absorbing 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 characteristics Therefore intensity spectra will differ slightly between instruments Figure 30 on page 101 shows a typical intensity test spectrum The Intensity Test is available in Agilent Lab Advisor preferred Agilent ChemStation Agilent Instant Pilot G4208A via More Diagnosis VWD Lamp Intensity Test Intensity Test Evaluation The Agilent LabAdvisor and the Instant Pilot evaluate three values automatically and display the limits for each value the average the minimum and the maximum of all data points and passed or failed for each value Agilent 1260 Infinity VWD User Manual Test Functions 8 Intensity Test Instensity Test with Agilent Lab Advisor Test Name Intensity Test Description The test scans the Intensity spectrum generated by the UV Module G1314CJP92110261 Crus Status Passed Start Time 5 9 2010 11 44 10 4M Stop Time 5 9 2010 11 44 49
60. ce slit reference diode Therefore the reference side value can be higher smaller than the sample side value With a clean cell the counts for sample and reference photocurrent are in the same range If the sample side shows much lower values than the reference side the flow cell might have a problem Pre requisite Flush the flow cell with a flow of 1 mL min for at least 10 minutes Probable Cause Suggested Action Cell contaminated Flush flow cell Cell windows are contaminated Clean replace cell windows Mechanical problem Check cell position In the Agilent Instant Pilot G4208A the photocurrent readings are available via More gt Diagnosis gt VWD gt Lamplntensity Test see Figure 32 on page 103 Agilent 1260 Infinity VWD User Manual Test Functions 8 Cell Test Test Name Cell Test Description Calculate the ratio of the sample signal and the reference signal measured in the zero order of the grating Module G1314C DE60555128 Status Passed Start Time 7 6 2011 1 24 55 PM Stop Time 7 6 2011 1 26 18 PM wc Test Procedure Result Name Value WY 1 Check Prerequistes Accumulated UV Lamp Burn Time 60 49 h 4 2 Fush Fow Cell UV Lamp On Time 436h 4 3 Measure Sample and Reference Intensity Intensity Sample 241 908 Counts WX Ede Intensity Reference 422 625 Counts RE Intensity Ratio 087 Figure 31 Cell Test with Lab Advisor Checking the Photocurrent with the Instant Pilot Diagnos
61. conformity 189 filler 13 test 110 HP JetDirect card 164 humidity 24 information on sound emission 185 on UV radiation 186 on cuvette holder 126 onsolvents 187 installation bench space 22 environment 23 of flow connections 42 site requirements 20 instrument layout 18 interface board replacing 130 interfaces 169 internet 190 introduction 10 to optical system 11 L lamp exchange 119 initial drift 58 intensity test 100 type 25 27 LAN cable 155 communication interface board 164 eak handling system parts replacing 129 eak sensor open 86 eak sensor short 87 eak correcting 128 parts 143 ine frequency 24 ine voltage 24 inearity 25 27 29 ithium batteries 183 ost CAN partner 85 M maintenance definition of 114 Agilent 1260 Infinity VWD User Manual for parts see parts for maintenance 133 introduction 113 overview 11 7 replacing firmware 131 131 using the cuvette holder 126 message ADC hardware error 96 calibration failed 93 calibration lost 95 filter check failed 96 grating filter motor defective 94 heater current missing 92 holmium oxide test failed 94 ignition without cover 89 89 lamp current missing 90 lamp ignition failed 91 lamp voltage missing 90 remote timeout 84 wavelength check failed 95 method load 54 mirror assemblies 14 noise short term 25 27 non operating altitude 24 non operating temperature 24 0 online plot 58 spectra 62 operating Altitude 24 operating
62. d to evaluate if the instrument is in good condition or damaged gt Notify your Agilent sales and service office about the damage gt An Agilent service representative will inspect the instrument at your site and initiate appropriate actions CAUTION Condensation Condensation within the detector Condensation will damage the system electronics Do not store ship or use your detector under conditions where temperature fluctuations could cause condensation within the detector f your detector was shipped in cold weather leave it in its box and allow it to warm up slowly to room temperature to avoid condensation 32 Agilent 1260 Infinity VWD User Manual Installing the Detector 3 Delivery Checklist Ensure all parts and materials have been delivered with the detector The delivery checklist is shown below Please report missing or damaged parts to your local Agilent Technologies sales and service office Table5 X Variable Wavelength Detector Checklist Description Quantity Variable wavelength detector 1 Power cable 1 Flow cell As ordered User Documentation DVD 1 Accessory kit see Accessory Kit on page 144 1 Detector Accessory Kit Contents The G1314B C VWD is shipped with Accessory kit p n G1314 68755 see Accessory Kit on page 144 Agilent 1260 Infinity VWD User Manual 33 3 Installing the Detector Optimizing the Stack Configuration 34 If your module is part of a complete
63. dback EMF for continuous tracking of instrument usage in terms of lamp burn time with user settable limits and feedback messages Electronic records of maintenance and errors Verification of wavelength accuracy with built in holmium oxide filter All materials recyclable 28 Agilent 1260 Infinity VWD User Manual Site Requirements and Specifications 2 Specification Conditions ASTM Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chromatography Reference conditions Standard flow cell path length 10 nm flow 1 mL min LC grade methanol Noise lt t 0 5 105 AU at 254 nm TC 2 s ASTM RT 2 2 TC Linearity Linearity is measured with caffeine at 265 nm The specifications are based on the standard lamp G1314 60100 and may be not achieved when other lamp types or aged lamps are used ASTM drift tests require a temperature change below 2 C hour 3 6 F hour over one hour period Our published drift specification 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 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 gt two hours ASTM
64. e and for GPC analyses Limits 100 4000 mAU Signal Polarity can be switched to negative if required Enable analysis when lamp is off if the VWD is not used in a dual detector setup lamp off the not ready condition is not stopping the analysis Scan Range Step Used for stop flow scanning see Scanning with the VWD on page 63 Signal Polarity Positive Negative Enable analysis when lamp is off Scan Range 120 to 400 nm Step 2 nm Restore Defaults Cancel Spectra Window Help Margin for negative Absorbance The higher the value the greater the baseline noise Set this value only if you expect negative absorbance greater than 100 mAU Agilent 1260 Infinity VWD User Manual 65 4 Using the Detector Peakwidth Settings Do not use peak width shorter than necessary see also Set the Detector Parameters on page 74 1 To change the Peakwidth settings select Setup Detector Signals 2 In the section Peakwidth Responsetime click on the drop down list 3 Change the Peakwidth according to your needs Ce Set up VWD Signal of Control fy Online Spectra 5 Mot Ready Information Help WD Signal System 2 Signal Wavelength 254 nm Peakwidth Responsetime gt O1min 2s 0 00125 min 0 033 a gt 0 00125 min 0 03 s gt O1min 2s Figure 26 Peakwidth Setting 66 Peakwidth enables you to select the peak
65. e Wavelength Verification Calibration is available in Agilent Lab Advisor preferred tool Agilent Instant Pilot G4208A via More Diagnosis VWD Calibration When to Calibrate the Detector The detector is calibrated at the factory and under normal operating conditions should not require recalibration However it is advisable to recalibrate after maintenance flow cell or lamp after repair of components in the optical unit after exchange of the optical unit or VWM board ataregular interval at least once per year for example prior to an Operational Qualification Performance Verification procedure and when chromatographic results indicate the detector may require recalibration Agilent 1260 Infinity VWD User Manual Test Functions Wavelength Verification Calibration Wavelength Verification Calibration with Agilent LabAdvisor Test Name Wavelength Calibration Module G1314C JP32110261 Approx Time 3 min Status Running BEHEREEREEREREEREEENEI r Test Procedure v 1 Check Prerequisites 2 Wavelength Verification ui 3 Calibrate Detector amp Wavelength Calibration verification results Test Name Wavelength Calibration Module G1314C JP32110261 Status Passed Start Time 6 2 2010 3 12 43 PM Stop Time 6 2 2010 3 21 33 PM Test Procedure 1 Check Prerequisites Wavelength Verification Calibrate Detector Do you want to calibrate the detec
66. e of consumables is necessary In the event of such a failure the red status indicator at the front of the module is switched on and an entry is written into the module logbook 82 Agilent 1260 Infinity VWD User Manual Error Information 7 General Error Messages General error messages are generic to all Agilent 1200 Infinity Series modules Timeout Error ID 0062 The timeout threshold was exceeded Probable cause Suggested actions 1 The analysis was completed successfully Check the logbook for the occurrence and and the timeout function switched off the source of a not ready condition Restart the module as requested analysis where required 2 Anot ready condition was present duringa Check the logbook for the occurrence and sequence or multiple injection run for a source of a not ready condition Restart the period longer than the timeout threshold analysis where required Agilent 1260 Infinity VWD User Manual 83 7 84 Error Information Shutdown Error ID 0063 An external instrument has generated a shutdown signal on the remote line The module continually monitors the remote input connectors for status signals A LOW signal input on pin 4 of the remote connector generates the error message Probable cause 1 Leak detected in another module with a CAN connection to the system 2 Leak detected in an external instrument with a remote connection to the system 3 Shut down in an external instrument w
67. eadiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines In addition PREPARE and START REQUEST may be issued The signal levels are defined as standard TTL levels 0 V is logic true 5 0 V is false fan out is 10 V e input load is 2 2 kOhm against 5 0 V and output are open collector type inputs outputs wired or technique All common TTL circuits operate with a 5 V power supply A TTL signal is defined as low or L when between 0 V and 0 8 V and high or H when between 2 0 V and 5 0 V with respect to the ground terminal Agilent 1260 Infinity VWD User Manual 173 12 Hardware Information Table 19 Remote Signal Distribution Pin Signal Description 1 DGND Digital ground 2 PREPARE L Request to prepare for analysis for example calibration detector lamp on Receiver is any module performing pre analysis activities 3 START L Request to start run timetable Receiver is any module performing run time 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 soon as possible for example
68. ect 5equence F8 T f Manual Filename RP DSCHEASM 150_01 D C Prefix Counter m Sample Parameters Location Vial 1 blank run if no entry Sample Name Isocratic test sample Sample Amount 0 Multiplier fi ISTD Amount o Dilution fi Comment Isocratic test sample 1 ul 30 70 H20 Acetonitrile 1 5 ml min n Bun Method OK Cancel Help Figure 19 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 Agilent 1260 Infinity VWD User Manual 59 4 Using the Detector Running the Sample and Verifying the Results To start a run select the menu item RunControl gt Run Method 2 This will start the modules and the online plot on the Agilent ChemStation will show the resulting chromatogram m u DAD1 A Sig 254 4 Ref 800 100 D41014 10 440003 D i S y E CT a a er T a ed ar i a a Ds a min Figure 20 Chromatogram with Isocratic Test Sample Information about using the Data Analysis functions can be obtained from the Using your ChemStation manual supplied with your system 60 Agilent 1260 Infinity VWD User Manual Using the Detector 4 Special Settings of the Detector In this chapter special settings of the detector are described Control Settings VB Set up WWD Signal X
69. edures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The volume of substances should be reduced to the minimum required for the analysis gt Do not operate the instrument in an explosive atmosphere WARNING Eye damage by detector light 9 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 off before removing it WARNING Electrical shock Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened gt Do not remove the cover of the module Only certified persons are authorized to carry out repairs inside the module Agilent 1260 Infinity VWD User Manual 115 9 Maintenance Personal injury or damage to the product Agilent is not responsible for any damages caused in whole or in part by improper use of the products unauthorized alterations adjustments or modifications 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 gt Use your Agilent products only in the manner described in the Agilent product user guides CAUTION Safety standards for external equipment gt If you connect e
70. ell removed If the test is OK exchange the flow cell components 3 Dirty or defective holmium oxide filter Run the holmium oxide filter test If the test fails contact your Agilent service representative 4 Optical misalignment Please contact your Agilent service representative 112 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual ee 9 099 Maintenance o o E e e e d Introduction to Maintenance 114 e Warnings and Cautions 115 Overview of Maintenance 117 Cleaning the Module 118 Exchanging a Lamp 119 Exchanging a Flow Cell 122 Repairing the Flow Cells 124 Using the Cuvette Holder 126 Correcting Leaks 128 Replacing Leak Handling System Parts 129 Replacing the Interface Board 130 Replacing the Module s Firmware 131 This chapter provides general information on maintenance and repair of the detector XE Agilent Technologies 113 9 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 There are no serviceable parts inside Do not open the module 114 Agilent 1260 Infinity VWD User Manual Maintenance 9 Warnings and Cautions WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety proc
71. er with cutoff filter Cutoff filter Figure 3 Filter Assembly Mirror Assemblies M1 and M2 The instrument contains two spherical mirrors M1 and M2 The beam adjustable is vertically and horizontally Both mirrors are identical Grating Assembly The grating separates the light beam into all its component wavelengths and reflects the light onto mirror 2 Beam Splitter Assembly The beam splitter splits the light beam One part goes directly to the sample diode The other part of the light beam goes to the reference diode 14 Agilent 1260 Infinity VWD User Manual Introduction to the Variable Wavelength Detector 1 Photo Diodes Assemblies Two photo diode assemblies are installed in the optical unit The sample diode assembly is located on the left side of the optical unit The reference diode assembly is located in the front of the optical unit Photo Diode ADC analog to digital converter The photo diode current is directly converted to digital data direct photo current digitalization The data is transferred to the detector main board The photo diode ADC boards are located close to the photo diodes Agilent 1260 Infinity VWD User Manual 15 1 Introduction to the Variable Wavelength Detector Early Maintenance Feedback EMF Maintenance requires the exchange of components which are subject to wear or stress Ideally the frequency at which components are exchanged should be based on the intensity of usage of t
72. er cord The power supply still uses Agilent 1260 Infinity VWD User Manual 41 3 Installing the Detector Flow Connections to the Detector Tools required Parts required Hardware required Preparations Description Wrench 1 4 5 16 inch p n Description 1 G1314 68755 Accessory kit Other modules depend on system setup Detector is installed in the LC system WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The volume of substances should be reduced to the minimum required for the analysis gt Do not operate the instrument in an explosive atmosphere 42 The flow cell is shipped with a filling of isopropanol also recommended when the instrument and or flow cell is shipped to another location This is to avoid breakage due to subambient conditions Agilent 1260 Infinity VWD User Manual 3 Installing the Detector 1 Press the release buttons and remove the front cover to have access to the lamp area 2 Remove the plastic dummy cover OR If the detector uses a metal plate loose the screws of the flow cell d
73. ested actions 1 Motor is not connected Please contact your Agilent service representative 2 Defective motor Please contact your Agilent service representative 3 Defective missing grating or filter Please contact your Agilent service representative 4 Cable connector defective Please contact your Agilent service representative Wavelength test failed Error ID 7890 The automatic wavelength check after lamp ignition has failed When the lamp is switched on the detector waits 1 min to warm up the lamp Then a check of the deuterium emission line 656 nm via the reference diode is performed If the emission line is more than 3 nm away from 656 nm the error message is generated Probable cause Suggested actions 1 Calibration incorrect Recalibrate the detector Agilent 1260 Infinity VWD User Manual 95 7 96 Error Information Cutoff filter doesn t decrease the light intensity at 250 nm Error ID 7813 The automatic filter check after lamp ignition has failed When the lamp is switched on the detector moves the cutoff filter into the light path If the filter is functioning correctly a decrease in lamp intensity is seen If the expected intensity decrease is not detected the error message is generated Probable cause Suggested actions 1 Motor is not connected Please contact your Agilent service representative 2 Defective motor Please contact your Agilent service representative 3 Defective missing grating o
74. ests n a n a Holmium Test Tests Tests Diagnosis Cell Test Tests Tests n a D A Converter Test Tests Tests n a Dark Current Test Tests Tests n a Filter Grating Motor Test Tests Tests n a Test Chromatogram Tools from command line n a Spectrum Blank Sample Holmium Tools n a n a interface provides passed fail information or a plot Agilent 1260 Infinity VWD User Manual 79 Troubleshooting and Diagnostics Agilent Lab Advisor Software 80 The Agilent Lab Advisor software is a standalone product that can be used with or without data system Agilent Lab Advisor software helps to manage the lab for high quality chromatographic results and can monitor in real time a single Agilent LC or all the Agilent GCs and LCs configured on the lab intranet Agilent Lab Advisor software provides diagnostic capabilities for all Agilent 1200 Infinity Series modules This includes diagnostic 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 as provided by the Agilent Lab Advisor software may differ from the descriptions in this manual For details refer to the Agilent Lab Advisor
75. ettings diagnosis and repair log books which will not be erased gt Save your methods and data before executing a forced cold start If you use the following switch settings and power the instrument up again a forced cold start has been completed Table 26 Forced Cold Start Settings without on board LAN Mode Select SW1 sw SW3 SW4 SW5 SW6 SW7 SW8 No LAN TEST BOOT 1 1 0 0 1 0 0 1 178 Agilent 1260 Infinity VWD User Manual This chapter provides addition information on safety legal and web Agilent 1260 Infinity VWD User Manual 13 Appendix General Safety Information 180 Batteries Information 183 Radio Interference 184 Sound Emission 185 UV Radiation 186 Solvent Information 187 Declaration of Conformity for HOX2 Filter 189 Agilent Technologies on Internet 190 RE Agilent Technologies 179 13 Appendix General Safety Information General Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument
76. fic for this purpose For other applications the system can be optimized in various ways Please refer to the section Optimizing the Detector Performance on page 70 50 Agilent 1260 Infinity VWD User Manual Using the Detector 4 Preparing the HPLC System 1 Turn on the Agilent ChemStation PC and the monitor 2 Turn on the modules 3 Start the Agilent ChemStation software If the pump autosampler thermostatted column compartment and detector are found the Agilent ChemStation screen should look like shown in Figure 11 on page 51 The System status is red Not Ready System status Method and Run Control LasRun M ee FUE mm DEF LC S EME Sane SO i9 ar I i FE exe Mo dd FO O e a RAR DEFAULT D LEE Lor Jot j no Details amp E data Ee E 1 1 GB free Online plot window details window Figure 11 Initial Agilent ChemStation screen Method and Run Control Agilent 1260 Infinity VWD User Manual 51 4 Using the Detector Method and Run Control see ST es ceric oe eercs EMG 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 SmO DEFAULT D Method and Run Control 0 bar D 0 000 ml min Last Run nares q
77. flow cell outside of the cell compartment and all capillary connections Insert the flow cell Perform Wavelength Verification Calibration on page 104 to check the correct positioning of the flow cell Replace the front cover Agilent 1260 Infinity VWD User Manual 123 9 Maintenance Repairing the Flow Cells When Tools required Parts required Preparations CAUTION If the flow cell needs repair due to leaks or contaminations Description Wrench 1 4 inch Wrench 4 mm hexagonal Toothpick Description See Standard Flow Cell 10 mm 14 pL on page 135 See Micro Flow Cell 5 mm 1 uL only for support on page 136 See Semi micro Flow Cell 6 mm 5 pL on page 140 See High Pressure Flow Cell 10 mm 14 uL on page 141 Turn off the flow Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 122 The shown cell parts will differ depending upon the flow cell type For detailed parts schematics refer to above mentioned pages Disassembling the Flow Cell 1 Unscrew the cell screw using a 4 mm hexagonal wrench 2 Remove the SST rings using a pair of tweezers Scratched window surfaces by tweezers Window surfaces can easily be scratched by using tweezers for removing the windows gt Do not use tweezers to remove windows 124 3 Use adhesive tape to remove the peek ring the window and the gasket 4 Repeat step 1 through step 3 for the other w
78. gh 5 15 Red 7 Ready High Green 8 Stop Low Black 9 Start request Low Agilent 1260 Infinity VWD User Manual Identifying Cables 11 BCD Cables One end of these cables provides a 15 pin BCD connector to be connected to the Agilent modules The other end depends on the instrument to be connected to Agilent Module to General Purpose p n G1351 81600 Wire Color Pin Agilent Signal Name BCD Digit module Green 1 BCD 5 20 Violet 2 BCD7 80 p 1 Blue 3 BCD 6 40 ERR Yellow 4 BCD 4 10 SS Black 5 BCD 0 1 MCN Orange 6 BCD 3 8 Red 7 BCD2 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 notconnected 14 notconnected 15 5V Low Agilent 1260 Infinity VWD User Manual 153 11 Identifying Cables Agilent Module to 3396 Integrators p n 03396 60560 Pin 3396 Pin Agilent Signal Name BCD Digit module n 1 1 BCD 5 20 ae 2 2 BCD 7 80 K 3 3 BCD 6 40 4 4 BCD 4 10 5 5 BCDO 1 6 BCD 3 8 z 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 154 Agilent 1260 Infinity VWD User Manual CAN LAN Cables Identifying Cables 11 Both ends of this cable provide a modular plug to be connected to Agilent modules CAN or LAN connectors CAN Cables p n 5181 1516 5181 1519 LAN Cables p n 5023 0203 5023 0202 Description CAN cable Agilent module to module 0
79. he instrument and the analytical conditions and not on a predefined time interval The early maintenance feedback EMF feature monitors the usage of specific components in the instrument and provides feedback when the user selectable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled EMF Counter The detector module provides a EMF counter for the lamp The counter increments with lamp use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded The counter can be reset to zero after the lamp is exchanged The detector provides the following EMF counters Deuterium Lamp On Time 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 lamp burn time is dependent on the requirements for the analysis high or low sensitivity analysis wavelength etc therefore the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument 16 Agilent 1260 Infinity VWD User Manual Introduction to the Variable Wavelength Detector 1 Setting the EMF Limits The setting of the EMF limits must be optimized over one or two maintenance cycles Initially no EMF limit should be set When instrument performance indicates maintenance is necessary
80. hnologies to ensure proper functionality and compliance with safety or EMC regulations Agilent 1260 Infinity VWD User Manual 21 2 Site Requirements and Specifications WARNING Unintended use of supplied power cords Using power cords for unintended purposes can lead to personal injury or damage of electronic equipment gt Never use the power cords that Agilent Technologies supplies with this instrument for any other equipment Bench Space The detector dimensions and weight see Physical Specifications on page 24 allows you to place the detector on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 inch of space on either side and approximately 8 cm 3 1 inch in the rear for air circulation and electric connections If the bench should carry an Agilent 1200 Infinity Series system make sure that the bench is designed to bear the weight of all modules The detector should be operated in a horizontal position 22 Agilent 1260 Infinity VWD User Manual Site Requirements and Specifications 2 Environment CAUTION Your detector will work within the specifications at ambient temperatures and relative humidity described in Physical Specifications on page 24 ASTM drift tests require a temperature change below 2 C h 3 6 F h over one hour period Our published drift specification refer also to Performance Specifications G1314B on page 25 or Performance Specifications G1
81. hronization or communication between one or more of the modules in the system has failed The system processors continually monitor the system configuration If one or more of the modules is no longer recognized as being connected to the system 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 module Switch off the system Restart the system and determine which module or modules are not recognized by the system Agilent 1260 Infinity VWD User Manual 85 7 86 Error Information Leak Error ID 0064 A leak was detected in the module The signals from the two temperature sensors leak sensor and board mounted temperature compensation 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 flow cell Exchange flow cell components Leak Sensor Open Error ID 0083 The leak sensor in the module has failed open circuit The current through the leak sensor is dependent
82. indow keep the parts separate otherwise they could be mixed Agilent 1260 Infinity VWD User Manual Maintenance 9 Cleaning the Flow Cell Parts 1 Pour isopropanol into the cell hole and wipe clean with a piece of lint free cloth 2 Clean the windows with ethanol or methanol Dry it with a piece of lint free cloth Always use new gaskets Reassembling the Flow Cell 1 Hold the flow cell cassette horizontally and place gasket in position Ensure both cell holes can be seen through the holes of gasket The semi micro 1 and 2 gaskets items 6 and 7 Semi micro Flow Cell 6 mm 5 uL on page 140 look very similar Do not mix them up 2 Place the window on gasket 3 Place the peek ring on the window 4 Insert the conical springs Make sure the conical springs point towards the window Otherwise tightening the cell screw might break the window Conical springs y Ring Window Gasket Arrangement Figure 38 Orientation of conical springs 5 Screw the cell screw into the flow cell and tighten the screw 6 Repeat the procedure for the other cell side Next steps 1 Reconnect the capillaries 2 Perform a leak test If OK insert the flow cell 3 Perform Wavelength Verification Calibration on page 104 to check the correct positioning of the flow cell 4 Replace the front cover Agilent 1260 Infinity VWD User Manual 125 9 Maintenance Using the Cuvette Holder This cuvette holder
83. instrumentation can result if the devices are connected to a line voltage higher than specified gt Connect your instrument to the specified line voltage only 20 Agilent 1260 Infinity VWD User Manual CAUTION Site Requirements and Specifications 2 Inaccessible power plug In case of emergency it must be possible to disconnect the instrument from the power line at any time gt Make sure the power connector of the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable Power Cords Different power cords are offered as options with the module The female end of all power cords is identical It plugs into the power input socket at the rear The male end of each power cord is different and designed to match the wall socket of a particular country or region Absence of ground connection or use of unspecified power cord The absence of ground connection or the use of unspecified power cord can lead to electric shock or short circuit gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region 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 Agilent Tec
84. is Intensity VWD SL Passed Max intens gt 320 000 cts measured 6039917 Min intens gt 6 400 cts measured 25507 Passed Avrg intens gt 160 000 cts measured 884724 Passed Finished Passed Y Figure 32 Checking the Photocurrent with the Instant Pilot Agilent 1260 Infinity VWD User Manual 103 Test Functions Wavelength Verification Calibration 104 Wavelength calibration of the detector is done using the zero order position and 656 nm emission line position of the deuterium lamp The calibration procedure involves two steps First the grating is calibrated on the zero order position The stepper motor step position where the zero order maximum is detected is stored in the detector Next the grating is calibrated against the deuterium emission line at 656 nm and the motor position at which the maximum occurs is stored in the detector In addition to the zero order and 656 nm alpha emission line calibration the beta emission line at 486 nm and the three holmium lines are used for the complete wavelength calibration process These holmium lines are at 360 8 nm 418 5 nm and 536 4 nm The wavelength verification calibration takes about 2 5 min and is disabled within the first 10 min after ignition of the lamp because initial drift may distort the measurement When the lamp is turned ON the 656 nm emission line position of the deuterium lamp is checked automatically Th
85. ith a remote connection to the system 4 The degasser failed to generate sufficient vacuum for solvent degassing Remote Timeout Error ID 0070 Suggested actions Fix the leak in the external instrument before restarting the module Fix the leak in the external instrument before restarting the module Check external instruments for a shut down condition Check the vacuum degasser for an error condition Refer to the Service Manual for the degasser or the 1260 pump that has the degasser built in A not ready condition is still present on the remote input When an analysis is started the system expects all not ready conditions for example a not ready condition during detector balance to switch to run conditions within one minute of starting the analysis If a not ready condition is still present on the remote line after one minute the error message is generated Agilent 1260 Infinity VWD User Manual Error Information 7 Probable cause Suggested actions 1 Not ready condition in one of the Ensure the instrument showing the not ready instruments connected to the remote line condition is installed correctly and is set up correctly for analysis 2 Defective remote cable Exchange the remote cable 3 Defective components in the instrument Check the instrument for defects refer to the showing the not ready condition instrument s documentation Lost CAN Partner Error ID 0071 During an analysis the internal sync
86. l Institute of Declaration of Conformi Holmium Oxide Glass Filter Standards and Technology NIST to be applied as certified wavelength standard According to the publication of NIST in J Res Natl Inst Stand Technol 112 303 306 2007 the holmium oxide glass filters are inherently stable with respect to the wavelength scale and need no recertification The expanded uncertainty of the certified wavelength values is 0 2 om Agilent Technologies guarantees as required by NIST that the material of the filters is holmium oxide glass representing the inherently existent holmium oxide absorption bands Test wavelengths Product Number 79883A 79854A G1306A Wavelength Optical Accuracy Bandwidth G1315A G1365A G1315B C G1365B C G1600A G7100A G1314A B C GI314D EF 4286 90A B C 1120 1220 The variation in Measured Wavelength depends on the different Optical Bandwidth P N 89550 90501 Agilent 1260 Infinity VWD User Manual May 19 2010 Revision H 3 Agilent Technologies ll Effective by May 19 2010 E 189 13 Appendix Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com Select Products Chemical Analysis It will provide also the latest firmware of the modules for download 190 Agilent 1260 Infinity VWD User Manual Index 8 bit configuration switch wi
87. ll the ESD strap Move the power lock across the 2 If required unscrew and remove the interface board power inlet Place the board on the ESD kit ESD strap x Ne v lt s P vB lt 7 4 X ist SA er E Es za j 22228 mic MW 2 v z S o o 2 KI S Next Steps 3 If required insert the interface board and fix the screws 4 Remove the ESD strap 5 Reinstall the module into the stack 130 Agilent 1260 Infinity VWD User Manual Maintenance 9 Replacing the Module s Firmware When 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 ifanew module with newer firmware is added to a system or ifthird part control software requires a special version Tools required Description LAN RS 232 Firmware Update Tool OR Agilent Diagnostic Software OR Instant Pilot G4208A Parts required Description 1 Firmware tools and documentation from Agilent web site Preparations Read update documentation provided with the Firmware Update Tool To upgrade downgrade the module s firmware carry out the following steps 1 Download the required module firmware the latest LAN RS 232 FW Update Tool and the documentation from the Agilent web http www chem agilent com scripts cag_firmware
88. ls G1314B G1314C Part number Path length actual Correction factor Standard flow cell 10 mm 14 uL 40 bar p n G1314 60086 10 15 0 19 mm 10 10 15 Semi micro flow cell 6 mm 5 pL 40 bar p n G1314 60083 6 10 0 19 mm 6 6 10 Micro flow cell without I D tag 3 mm 2 uL 120 bar p n G1314 60087 2 80 0 19 mm 3 2 80 High pressure flow cell 10 mm 14 pL 400 bar p n G1314 60082 10 00 0 19 mm 10 10 However you have to be aware that there are additional tolerance of gasket thickness and its compression ratio which is supposed to be very small in comparison with the machining tolerance Agilent 1260 Infinity VWD User Manual 73 5 How to optimize the detector Set the Detector Parameters 1 Set peakwidth as close as possible to the width at half height of a narrow peak of interest Refer to Peakwidth Settings on page 66 2 Choose the sample wavelength at a longer wavelength than the cut off wavelength of the mobile phase at a wavelength where the analytes have strong absorptivity if you want to get the lowest possible detection limit at a wavelength with moderate absorptivity if you work with high concentrations and preferably where the spectrum is flat for better linearity 3 Consider to use time programming to further optimization 74 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual 6 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functi
89. m 14uL 141 Cuvette Holder 142 Leak Parts 143 Kits 144 1 Identifying Cables 145 Cable Overview 146 Analog Cables 148 Remote Cables 150 BCD Cables 153 CAN LAN Cables 155 RS 232 Cable Kit 156 External Contact Cable 157 12 Hardware Information 159 Firmware Description 160 Optional Interface Boards 163 Electrical Connections 166 Interfaces 169 Setting the 8 bit Configuration Switch without On board LAN 175 13 Appendix 179 General Safety Information 180 Batteries Information 183 Radio Interference 184 Sound Emission 185 UV Radiation 186 Solvent Information 187 Declaration of Conformity for HOX2 Filter 189 Agilent Technologies on Internet 190 Agilent 1260 Infinity VWD User Manual Contents 8 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual EUR to the Variable Wavelength e e e9 e eo 0e Qeu9 Detector e Introduction to the Detector 10 Optical System Overview 11 Flow Cell 12 G1314B C Lamp 13 Source Lens Assembly 13 Entrance Slit Assembly 13 Filter Assembly 13 Mirror Assemblies M1 and M2 14 Grating Assembly 14 Beam Splitter Assembly 14 Photo Diodes Assemblies 15 Photo Diode ADC analog to digital converter 15 Early Maintenance Feedback EMF 16 EMF Counter 16 Using the EMF Counters 16 Instrument Layout 18 This chapter gives an introduction to the detector instrument overview and internal connectors Agilent Technologies 9
90. mage Indicates dangerous voltages Indicates a protected ground terminal Indicates eye damage may result from directly viewing the light produced Z 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 UMS 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 conditions CAUTION A CAUTION alerts you to situations that could cause loss of data or damage of equipment Do not proceed beyond a caution until you have fully understood and met the indicated conditions 182 Agilent 1260 Infinity VWD User Manual Appendix 13 Batteries Information Lithium batteries may not be disposed off into the domestic waste Transportation of discharged Lithium batteries through carriers regulated by IATA ICAO ADR RID IMDG is not allowed Danger of explosion if battery is incorrectly replaced gt Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries Replace only with the same or equivalent type recommended by the equipment manufacturer Lithiumbatteri Eksplosionsfare ved fejlagtig handtering Udskiftning m kun ske med batteri af samme fabrikat og type Lever det brugte batteri tilbage til leverandgren Lithiumba
91. measurements require that the detector should be turned on at least 24 hours before start of testing Time Constant versus Response Time According to ASTM E1657 98 Standard Practice of Testing Variable Wavelength Photometric Detectors Used in Liquid Chromatography the time constant is converted to response time by multiplying by the factor 2 2 Agilent 1260 Infinity VWD User Manual 29 2 Site Requirements and Specifications Performance Specifications 30 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual 3 Installing the Detector Unpacking the Detector 32 Unpacking the Detector 32 Delivery Checklist 33 Detector Accessory Kit Contents 33 Optimizing the Stack Configuration 34 One Stack Configuration 34 Two Stack Configuration 37 Installing the Detector 39 Flow Connections to the Detector 42 This chapter provides information on unpacking checking on completeness stack considerations and installation of the module RE Agilent Technologies 31 3 Installing the Detector Unpacking the Detector CAUTION Damaged Packaging If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your service representative that the instrument may have been damaged during shipment Defective on arrival problems If there are signs of damage please do not attempt to install the module Inspection by Agilent is require
92. ns to the Detector on page 42 4 Connect the power cable to the power connector at the rear of the detector 5 Connect the CAN cable to other Agilent 1260 Infinity modules 6 Ifa Agilent ChemStation is the controller connect the LAN connection to the LAN interface board in the detector If an Agilent 1200 Infinity Series DAD MWD FLD is in the system the LAN should be connected to the DAD MWD FLD due to higher data load 7 Connect the analog cable optional 8 Connect the APG remote cable optional for non Agilent 1260 Infinity instruments 40 Agilent 1260 Infinity VWD User Manual Installing the Detector 3 Installing the Detector 9 Turn ON power by pushing the button at the lower left hand side of the detector The status LED should be green Security lever Interface board O00000 Analog signal APG Remote RS 232C CAN Configuration switch Power Figure 9 Rear View of Detector NOTE The detector is turned ON when the line power switch is pressed and the green indicator lamp is illuminated The detector is turned OFF when the line power switch is protruding and the green light is OFF some power even if the power switch at the front panel is turned OFF NOTE The detector was shipped with default configuration settings To change these settings see Setting the 8 bit Configuration Switch without On board LAN on page 175 NOTE To disconnect the detector from line unplug the pow
93. nt 35900 A D converters or HP 1050 1046A 1049A 01046 60201 Agilent module to general purpose BCD cables p n Description 03396 60560 Agilent module to 3396 integrators G1351 81600 Agilent module to general purpose Agilent 1260 Infinity VWD User Manual Identifying Cables 11 CAN 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 LAN cables 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 External Contact Cable p n Description G1103 61611 External contact cable Agilent module interface board to general purposes RS 232 cables p n Description G1530 60600 RS 232 cable 2 m RS232 61600 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 Agilent 1260 Infinity VWD User Manual 147 11 Identifying Cables Analog Cables 148 eC JEJSIOO 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 Integra
94. o helps to reduce or eliminate radio frequency emissions from the instrument itself 18 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual ee 2 Site Requirements and Specifications o o E e e i e i Site Requirements 20 e Physical Specifications 24 Performance Specifications 25 Specification Conditions 29 This chapter gives information on environmental requirements physical and performance specifications RE Agilent Technologies 2 Site Requirements and Specifications Site Requirements Site Requirements A suitable environment is important to ensure optimal performance of the instrument Power Consideration The detector power supply has wide ranging capabilities see Physical Specifications on page 24 It accepts any line voltage in the above mentioned range Consequently there is no voltage selector in the rear of the detector There are also no externally accessible fuses because automatic electronic fuses are implemented in the power supply Instrument is partially energized when switched off The power supply still uses some power even when the power switch on the front panel is turned OFF Repair work at the detector can lead to personal injuries e g shock hazard when the detector cover is opened and the instrument is connected to power gt To disconnect the detector from the power line unplug the power cord Hazard of electrical shock or damage of your
95. ons 76 Status Indicators 77 Power Supply Indicator 77 Module Status Indicator 78 Available Tests versus Interfaces 79 Agilent Lab Advisor Software 80 Overview about the troubleshooting and diagnostic features RE Agilent Technologies 75 6 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functions Status Indicators The detector is provided with two status indicators which indicate the operational state prerun run and error states of the detector The status indicators provide a quick visual check of the operation of the detector Error Messages In the event of an electronic mechanical or hydraulic failure the detector generates an error message in the user interface 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 Test Functions A series of test functions are available for troubleshooting and operational verification after exchanging internal components Wavelength Verification Recalibration Wavelength recalibration is recommended after repair of internal components and on a regular basis to ensure correct operation of the detector The detector uses the deuterium alpha and beta emission lines for wavelength calibration Diagnostic Signals The detector has several signals internal temperatures voltages and currents of lamps that can be used for diagnosing baseline pro
96. r information 167 167 193 Index setting up an analysis 46 settings analog output settings 64 peakwidth 66 setup of detector 55 shutdown 84 signal diagnostic 76 plot 57 site requirements 20 power cords 21 power considerations 20 solvent information 187 sound emission 185 source lens assembly 13 special interfaces 174 special setpoints 65 special settings boot resident 178 forced cold start 178 specification physical 24 specifications physical 24 spectra online 62 stack configuration 38 rearview 38 status indicators 76 status indicator 78 stop flow condition 62 system setup and installation optimizing stack configuration 34 T temperature sensor 86 test functions 76 99 tests available tests vs interface 79 194 dark current 108 holmium oxide 110 intensity of deuterium lamp 100 wavelength calibration 104 test Quick Noise 107 timeout 83 tool kit hplc system 144 troubleshooting available tests vs interface 79 diagnostic signals 76 error messages 82 76 overview 76 status indicators 76 77 test functions 99 76 U unpacking 32 using analog output settings 64 detector parameters 55 EMF 16 load method 54 online plot 58 online spectra 62 peakwidth settings 66 preparing the HPLC system 51 priming and purging the system 46 requirements and conditions 48 running the sample 60 sample info 59 setting up an analysis 46 setup of detector 55 signal plot 57 speci
97. r filter Please contact your Agilent service representative 4 Cable connector defective Please contact your Agilent service representative ADC Hardware Error Error ID 7830 7831 A D Converter hardware is defective Probable cause Suggested actions 1 A D Converter hardware is defective Please contact your Agilent service representative Agilent 1260 Infinity VWD User Manual Error Information 7 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 Please contact your Agilent service representative 2 Foam not activating the sensor Please contact your Agilent service representative Agilent 1260 Infinity VWD User Manual 97 7 Error Information Detector Error Messages 98 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual 8 Test Functions Intensity Test 100 Intensity Test Failed 101 Cell Test 102 Wavelength Verification Calibration 104 ASTM Drift and Noise Test 106 Quick Noise Test 107 Dark Current Test 108 Dark Current Test Failed 108 Holmium Oxide Test 110 Holmium Oxide Test Failed 112 This chapter describes the detector s
98. r repair Interpreting the Results The test is passed successfully when all three wavelengths are within 1 nm of the expected value This indicates the detector is calibrated correctly ChemStation revisions below B 01 xx show a limit of 2 nm It should read 1 nm If the test shows a value greater than 1 nm perform a recalibration Agilent 1260 Infinity VWD User Manual Test Functions 8 Holmium Oxide Test Running the test with Agilent Lab Advisor Test Name Holmium Oxide Test Description The test measures the Holmium spectrum from the built in Holmium filter The spectrum is evaluated for peaks at different Module G1314C JP32110261 wavelengths Status Passed Start Time 6 2 2010 3 40 32 PM Stop Time 6 2 2010 3 43 14 PM r Test Procedure Result Name falue M 1 Check Prerequisites Accumulated UV Lamp Burn Time 32 87 h V 2 Perform Holmium Oxide Test UV Lamp On Time amp 3 Evaluate Data Holmium Deviation to 360 8 nm 2 00rnm Holmium Deviation to 418 5 nm Onm Holmium Deviation to 536 4 nm 00nm Absorbance AU 5 3754 0 075038 1 1 T 190 400 500 800 Wavelength nm Figure 37 Holmium Test with Agilent Lab Advisor Agilent 1260 Infinity VWD User Manual 111 8 Test Functions Holmium Oxide Test Failed Probable cause Suggested actions 1 Detector not calibrated Recalibrate the detector 2 Dirty or defective flow cell Repeat the test with the flow c
99. ritten agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance 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 subcon tract 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 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to could result in damage to the p
100. rmation on how to set up the detector for an analysis and explains the basic settings Agilent Technologies 45 4 Using the Detector Setting up an Analysis 46 This chapter can be used for preparing the system tolearn the set up of an HPLC analysis and to use it as an instrument check to demonstrate that all modules of the system are correctly installed and connected It is not a test of the instrument performance Learn about special settings All descriptions are based on the Agilent ChemStation B 02 01 Newer versions may look different Before Using the System Solvent Information Observe recommendations on the use of solvents in chapter Solvents in the pump s reference manual 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 Solvents containing volatile ingredients will slightly lose these Therefore priming of the pumping system is required before starting an application Agilent 1260 Infinity VWD User Manual Table 6 Choice of Priming Solvents for Different Purposes Using the Detector 4 Activity Solvent Comments After an installation Isopropanol Best solvent to flush air out of the system When switching between reverse Isopropanol Best sol
101. roduct or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met Agilent 1260 Infinity VWD User Manual In This Guide In This Guide This manual covers the Agilent 1260 Infinity Variable Wavelength Detectors G1314B Agilent 1260 Infinity Variable Wavelength Detector VL e G1314C Agilent 1260 Infinity Variable Wavelength Detector VL 1 Introduction to the Variable Wavelength Detector This chapter gives an introduction to the detector instrument overview and internal connectors 2 Site Requirements and Specifications This chapter gives information on environmental requirements physical and performance specifications 3 Installing the Detector This chapter provides information on unpacking checking on completeness stack considerations and installation of the 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 chapter gives hints on how to select the detector parameters and the flow cell 6 Troubleshooting and Diagnostic
102. s WD Signal System 2 254 pOlmn 23 x Figure 16 Detector Settings default 56 1 signal with individual wavelength setting stop and post time can be set if required peakwidth depends on the peaks in the chromatogram see Peakwidth Settings on page 66 time table for programmable actions during the run Zero Offset Limits 1 99 in steps of 1 96 Attenuation Limits 0 98 4000 mAU at discrete values for either 100 mV or 1 V full scale additional signals can be stored with the normal signal for diagnostics autobalance to zero absorbance on the analog output plus offset at begin and or end of run see Special Setpoints on page 65 Agilent 1260 Infinity VWD User Manual Using the Detector 4 11 Pump the water acetonitrile 30 70 mobile phase through the column for 10 minutes for equilibration 12 Click the button and select Change to open the Signal Plot information Select the Pump Pressure and the VWD A Signal 254 as signals Change the Y range for the VWD to 1 mAU and the offset to 20 6 and the pressure offset to 50 The X axis range should be 15 minutes Press OK to exit this screen DEFAULT D Edit Signal Plot Selected Signals Available Signals Flow oR AB oC uaternary Pump 96D column Thermostat Temperature column Thermostat Temperature ri WD B Signal w o Reference at 254 x E AdataV zd E 1 1 GB free
103. s Overview about the troubleshooting and diagnostic features Agilent 1260 Infinity VWD User Manual 3 In This Guide 7 Error Information This chapter describes the meaning of detector error messages and provides information on probable causes and suggested actions how to recover from error conditions 8 Test Functions This chapter describes the detector s built in test functions 9 Maintenance This chapter provides general information on maintenance and repair of the detector 10 Parts and Materials for Maintenance This chapter provides information on parts for maintenance 11 Identifying Cables This chapter provides information on cables used with the Agilent 1260 Infinity modules 12 Hardware Information This chapter describes the detector in more detail on hardware and electronics 13 Appendix This chapter provides addition information on safety legal and web Agilent 1260 Infinity VWD User Manual Contents Contents 1 Introduction to the Variable Wavelength Detector 9 Introduction to the Detector 10 Optical System Overview 11 Early Maintenance Feedback EMF 16 Instrument Layout 18 2 Site Requirements and Specifications 19 Site Requirements 20 Physical Specifications 24 Performance Specifications 25 3 Installing the Detector 31 Unpacking the Detector 32 Optimizing the Stack Configuration 34 Installing the Detector 39 Flow Connections to the Detector 42 4 Using the Detector 45
104. software help files The Instrument Utilities is a basic version of the Lab Advisor with limited functionality required for installation use and maintenance No advanced repair troubleshooting and monitoring functionality is included Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual e o o o eee p Information a e e e What Are Error Messages 82 e General Error Messages 83 Timeout 83 Shutdown 84 Remote Timeout 84 Lost CAN Partner 85 Leak 86 Leak Sensor Open 86 Leak Sensor Short 87 Compensation Sensor Open 87 Compensation Sensor Short 88 Fan Failed 88 OpenCover 89 Detector Error Messages 90 UV lamp no current 90 UV lamp no voltage 90 Ignition Failed 91 No heater current 92 Wavelength calibration setting failed 93 Wavelength holmium check failed 94 Grating or Filter Motor Errors 94 Wavelength test failed 95 Cutoff filter doesn t decrease the light intensity at 250 nm 96 ADC Hardware Error 96 Cover Violation 97 This chapter describes the meaning of detector error messages and provides information on probable causes and suggested actions how to recover from error conditions Agilent Technologies 81 7 Error Information What Are Error Messages Error messages are displayed in the user interface when an electronic mechanical or hydraulic flow path failure occurs which requires attention before the analysis can be continued for example repair or exchang
105. ssory kit p n G1314 68755 contains some accessories and tools needed for installation and repair of the module p n Description 0100 1516 Fitting male PEEK 2 pk 5062 8535 Waste accessory kit PEEK capillary 0 25 mm i d 1 16 o d 500 mm long plus 2 MT PTFE tubing i d 0 8 m 1 16 o d 5063 6527 Tubing assembly i d 6 mm o d 9 mm 1 2 m to waste 5181 1516 CAN cable Agilent module to module 0 5 m 144 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual 11 Identifying Cables Cable Overview 146 Analog Cables 148 Remote Cables 150 BCD Cables 153 CAN LAN Cables 155 RS 232 Cable Kit 156 External Contact Cable 157 This chapter provides information on cables used with the Agilent 1260 Infinity modules E Agilent Technologies 145 11 Identifying Cables Cable Overview 146 Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Analog cables p n Description 35900 60750 Agilent module to 3394 6 integrators 35900 60750 Agilent 35900A A D converter 01046 60105 Analog cable BNC to general purpose spade lugs Remote cables p n Description 03394 60600 Agilent module to 3396A Series integrators 3396 Series Il 3395A integrator see details in section Remote Cables on page 150 03396 61010 Agilent module to 3396 Series III 3395B integrators 5061 3378 Agilent module to Agile
106. st performs ASTM Drift and Noise evaluation without fi k Module 81314C JP32110261 EEEN Status Passed Start Time 6 9 2010 12 13 54 PM Stop Time 6 9 2010 12 34 04 PM m Test Procedure Result M Sa Sa ae t Load cd m 7aT6h AY 2 Measure Noise UV Lamp On Time 1 83h 3 Evaluate Data Signal Drift value at 254 nm UY 0 043 mAU h Signal Noise value at 254 nm UV 0 006 m amp U Absorbance mAU 1 2412 1 245 1 25 1 255 1 2598 4 j I 0 e 4 6 10 12 Time min Figure 34 ASTM Drift and Noise Test Agilent Lab Advisor 106 Agilent 1260 Infinity VWD User Manual Test Functions 8 Quick Noise Test Quick Noise Test The noise test measures the noise of the detector with HPLC grade water flowing through the flow cell at 1 mL min in one minute intervals over a total of 5 min The noise of the detector is calculated by using the maximum amplitude for all random variations of the detector signal of frequencies greater than one cycle per hour The noise is determined for 5 one minute intervals and is based on the accumulated peak to peak noise for the intervals At least seven data points per cycles are used in the calculation The cycles in the noise determination are not overlapping In order to obtain reliable results the lamp should be turned on for at least 10 min prior to measurement Test Name Quick Noise Test Description The test performs a quick Noise Evaluation without reference Module G1314C JP92
107. tative Please contact your Agilent service representative 93 7 94 Error Information Wavelength holmium check failed Error ID 7318 The holmium oxide test in the detector has failed During the holmium test the detector moves the holmium filter into the light path and compares the measured absorbance maxima of the holmium oxide filter with expected maxima If the measured maxima are outside the limits the error message is generated Probable cause Suggested actions 1 Misaligned defective grating assembly Ensure the flow cell is inserted correctly and is free from contamination cell windows buffers and so on Run the filter motor test to determine if the filter motor assembly is defective If defective please contact your Agilent service representative Run the grating motor test to determine if the grating assembly is defective If defective please contact your Agilent service representative Grating or Filter Motor Errors Error ID Grating 7800 7801 7802 7803 7804 7805 7806 7808 7809 Filter 7810 7811 7812 7813 7814 7815 7816 The motor test has failed Test 0 Failed Filter motor Test 1 Failed Grating motor During the motor tests the detector moves the motor to the end position while monitoring the end position sensor If the end position is not found the error message is generated Agilent 1260 Infinity VWD User Manual Error Information 7 Probable cause Sugg
108. temperature 24 optical unit flow cell 12 optical unit beam splitter assembly 14 entrance slit assembly 13 filter assembly 13 filter 13 grating assembly 14 lamp 13 mirrors 14 photodiode assemblies 15 photodiode boards 15 source lens assembly 13 optimization detector performance 70 of the system 50 stack configuration 34 overview optical path 11 optical system 11 system overview 11 P packaging damaged 32 parameter setting 74 parameters detector 50 parts for maintenance cuvette holder 142 high pressure flow cell 141 leak parts 143 overview of maintenance parts 134 standard flow cell 135 parts and materials for maintenance 133 peakwidth settings 66 performance optimization 70 photodiode assemblies 15 boards 15 Agilent 1260 Infinity VWD User Manual Index photometric accuracy 73 physical specifications 24 physical specifications 24 power consumption 24 power cords 21 power considerations 20 preparing the HPLC system 51 radio interference 184 recalibration of wavelength 76 reference conditions 29 remote cable 150 repairs cautions and warnings 115 overview of simple repairs 117 replacing firmware 131 131 RS 232C cable 156 communication settings 176 running the sample 60 S safety class 180 safety information lithium batteries 183 safety general information 180 standards 24 symbols 182 sample info 59 scanning 63 semi micro flow cell parts 140 serial numbe
109. the larger flow cell to get the best detection limit Use the smaller flow cell for best peak resolution Standard HPLC Applications Column length T ypical peak width Recommended flow cell 0 025 min Micro flow cell Semimiro owca gt 40 om Typical flow rate 0 05 0 2 ml min 0 2 0 4 ml min 0 4 0 8 ml min 1 2 ml min 0 01 5 ml min Internal column diameter o O O Figure 27 Choosing a Flow Cell Standard HPLC Applications Agilent 1260 Infinity VWD User Manual 7 5 72 How to optimize the detector Flow Cell Path Length Lambert Beer s law shows a linear relationship between the flow cell path length and absorbance Absorbance log T log exCxd where T is the transmission defined as the quotient of the intensity of the transmitted light divided by the intensity of the incident light lg e is the extinction coefficient which is a characteristic of a given substance under a precisely defined set of conditions of wavelength solvent temperature and other parameters C mol L is the concentration of the absorbing species d cm 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 28 on page 73 the noise increased by less than 10 but a 70 increase in signal intensity was achieved by increasing
110. thout On Board LAN 175 A absorbance Beer Lambert 72 accessory kit content 33 Agilent Diagnostic software 80 Agilent Lab Advisor software 80 Agilent Lab Advisor 80 Agilent oninternet 190 algea information 187 ambient non operating temperature 24 ambient operating temperature 24 analog signal 172 analog cable 148 output range 64 output settings 64 apgremote 1 3 ASTM Drift and Noise Test 106 reference and conditions 29 B band width 6 5 nm 25 27 battery safety information 183 BCD board external contacts 163 BCD cable 153 beam splitter 14 Beer Lambert absorbance 72 benchspace 22 board HP JetDirect card 164 boards LAN card 164 photodiode boards ADC 15 C cable analog 148 BCD 153 CAN 155 connecting APG remote 38 connecting CAN 38 connecting LAN 38 connecting the ChemStation 38 connecting the power 38 external contact 157 LAN 155 remote 150 RS 232 156 cables analog 146 BCD 146 CAN 147 external contact 147 LAN 147 overview 146 remote 146 RS 232 147 CAN Agilent 1260 Infinity VWD User Manual Index cable 155 cautions and warnings 115 cell test 102 chromatogram 50 cleaning 118 Communication settings RS 232C 176 compensation sensor open 87 compensation sensor short 88 condensation 23 configuration one stack 34 34 two stack 37 correction factors for flow cells 73 cutoff filter 13 cuvette holder 126 parts 142 D dark current test 108 declaration of conformit
111. tor using the wavelength Description This procedure performs a Wavelength Verification and Recalibration Result Name Value Accumulated UY Lamp Burn Time 3241h UV Lamp On Time 0 36 h Time to Wait Before Wavelength Calibration 0 00 min Wavelength Gap of previous D order Calibra D 200 nm Maximum Wavelength Gap of previous Calib 0 200 nm Wavelength Gap of 0 order Calibration 0 400 nm Maximum Wavelength Gap of Calibration 0 300 nm x Description This procedure performs a Wavelength Verification and Recalibration Result Name Value Accumulated UY Lamp Burn Time 32 41h UV Lamp On Time 0 36 h Time to Wait Before Wavelength Calibration 0 00 min Wavelength Gap of previous order Calibra D 200 nm Maximum Wavelength Gap of previous Calib 0 200 nm Wavelength Gap of 0 order Calibration 0 400 nm Maximum Wavelength Gap of Calibration 0 300 nm Calibrate Detector with Wavelength Verificati Yes Figure 33 Wavelength Verification and Calibration Agilent Lab Advisor Agilent 1260 Infinity VWD User Manual 105 8 Test Functions ASTM Drift and Noise Test ASTM Drift and Noise Test The ASTM Drift and Noise test determines the detector noise over a period of 20 min The test is done with HPLC grade water flowing through the flow cell at 1 mL min On completion of the test the noise result is displayed automatically Test Name ASTM Drift and Noise Test Description The te
112. tors p n 35900 60750 Pin 3394 6 Pin Agilent Signal Name module 1 Not connected 2 Shield Analog 3 Center Analog To uri oO Agilent Module to BNC Connector p n 8120 1840 Pin BNC Pin Agilent Signal Name module Ml Sy Shield Shield Analog ad Center Center Analog Agilent 1260 Infinity VWD User Manual Agilent Module to General Purpose Identifying Cables 11 p n 01046 60105 Pin Pin Agilent Signal Name module 1 Not connected 2 Black Analog 3 Red Analog _ a Agilent 1260 Infinity VWD User Manual 149 11 Identifying Cables Remote Cables 150 One end of these cables provides a Agilent Technologies APG Analytical Products Group remote connector to be connected to Agilent modules The other end depends on the instrument to be connected to Agilent Module to 3396A Integrators p n 03394 60600 Pin 3396A Pin Agilent Signal Name Active module TTL 9 1 White Digital ground NC 2 Brown Prepare run Low 80 i 3 3 Gray Start Low E o NC 4 Blue Shut down Low o e e i NC 5 Pink Not connected le NC 6 Yellow Power on High 5 14 7 Red Ready High 1 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent Module to 3396 Series II 3395A Integrators Use the cable Agilent module to 3396A Series I integrators p n 03394 60600 and cut pin 5 on
113. tteri Eksplosionsfare Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten gt Brukt batteri returneres appararleverandoren Bij dit apparaat zijn batterijen geleverd Wanneer deze leeg zijn moet u ze niet weggooien maar inleveren als KCA Agilent 1260 Infinity VWD User Manual 183 13 Appendix Radio Interference Cables supplied by Agilent Technologies are screened to provide optimized protection against radio interference All cables are in compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with unscreened cables 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 184 Agilent 1260 Infinity VWD User Manual Appendix 13 Sound Emission Manufacturer s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position lt 70 dB Sound Pressure Lp lt 70 dB A At Operator Position Normal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test Agilent 1260 Infinity VWD User Manual 185 13 Appendix UV Radiation 186 Emissions of ultraviolet radiation 200 315 nm from this product is limited such that radiant exposure incident upon the unprotected skin or eye of operator
114. ummy plate by turning each screw one turn Then unscrew the screws completely This is required to avoid any problem with helicoil insert in the casting 3 Press the flow cell completely into the slot and tighten the cell screws both parallel until the mechanical stop 4 Assemble the column detector capillary Depending on the flow cell type it may be a PEEK or SST capillary Agilent 1260 Infinity VWD User Manual 43 3 Installing the Detector 5 Connect the newly assembled fitting of the capillary to 6 Connect the PEEK waste capillary to the outlet connector the inlet connector and connect the other end of the capillary to the column 8 Replace the front cover The installation of the detector is now complete The detector should be operated with the front cover in place to protect the flow cell area against strong drafts from the outside 44 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual rani the Detector Setting up an Analysis 46 Before Using the System 46 Requirements and Conditions 48 Optimization of the System 50 Preparing the HPLC System 51 Running the Sample and Verifying the Results 60 Special Settings of the Detector 61 Control Settings 61 Online Spectra 62 Scanning with the VWD 63 Analog Output Settings 64 Special Setpoints 65 This chapter provides info
115. under voltage should be avoided whenever possible When inevitable this has to be carried out by a skilled person who is aware of the hazard 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 make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting When working with solvents observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used Agilent 1260 Infinity VWD User Manual 181 13 Appendix Safety Symbols Table 27 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the N instruction manual in order to protect risk of harm to the operator and to protect the apparatus against da
116. uterium lamp 190 600 nm t 0 510 AU at 254 nm 3 10 AU h at 254 nm gt 2 AU 5 upper limit tinm 55 Hz 6 5 nm typical Standard 14 pL volume 10 mm cell path length and 40 bar 580 psi pressure maximum High pressure 14 pL volume 10 mm cell path length and 400 bar 5800 psi pressure maximum Micro 1 pL volume 5 mm cell path length and 40 bar 580 psi pressure maximum Semi micro 5 pL volume 6 mm cell path length and 40 bar 580 psi pressure maximum Agilent ChemStation for LC See Specification Conditions on page 29 See Specification Conditions on page 29 See Specification Conditions on page 29 Self calibration with deuterium lines verification with holmium oxide filter Can be repaired on component level Agilent 1260 Infinity VWD User Manual 27 2 Site Requirements and Specifications Table4 Performance Specifications G1314C Type Specification Comments Analog outputs Communications Safety and maintenance GLP features Housing Recorder integrator 100 mV or 1 V output range 0 001 to 2 AU one output Controller area network CAN RS 232C APG Remote ready start stop and shut down signals LAN optional Extensive diagnostics error detection and display through Agilent ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas Early maintenance fee
117. vent to flush air out of the phase and normal phase both times After an installation To clean the system when using buffers After a solvent change After the installation of normal phase seals P N 0905 1420 Ethanol or Methanol Bidistilled water Bidistilled water Hexane 5 Isopropanol system Alternative to Isopropanol second choice if no Isopropanol is available Best solvent to re dissolve buffer crystals Best solvent to re dissolve buffer crystals Good wetting properties The pump should never be used for priming empty tubings never let the pump run dry Use a syringe to draw enough solvent for completely filling the tubings to the pump inlet before continuing to prime with the pump 1 Open the purge valve of your pump by turning it counterclockwise and set flow rate to 3 5 mL min 2 Flush all tubes with at least 30 mL of solvent 3 Setflow to required value of your application and close the purge valve Pump for approximately 10 minutes before starting your application Agilent 1260 Infinity VWD User Manual 47 4 48 Using the Detector Requirements and Conditions What You Will Need The table below lists the items you need to have for the set up of the analysis Some of these are optional not required for the basic system Table 7 What you will need Agilent 1200 Infinity Series system Column Standard Pump plus degassing Autosampler Detector st
118. width response time for your analysis The peak width is defined as the width of a peak in minutes at half the peak height Set the peak width to the narrowest expected peak in your 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 setting of the peak width The time specified by the peak width is used as a factor in the acquisition of spectra The acquisition time for one spectrum is slightly less than the peak width divided by 8 see Table 9 on page 67 and Table 10 on page 67 Limits When you set the peak width in minutes the corresponding response time is set automatically and the appropriate data rate for signal acquisition is selected as shown in Table 9 on page 67 and Table 10 on page 67 Agilent 1260 Infinity VWD User Manual Using the Detector 4 Table9 Peak Width Response Time Data Rate G1314B VWD Peak Width min Response Time s Data Rate Hz lt 0 005 0 12 13 74 gt 0 005 0 12 13 74 gt 0 01 0 25 13 74 gt 0 025 0 5 13 74 gt 0 05 1 0 6 87 gt 0 10 2 0 3 43 gt 0 20 4 0 172 20 40 8 0 0 86 Values in the User Interface may be rounded Table 1
119. xternal Contact Cable 158 Agilent 1260 Infinity VWD User Manual Agilent 1260 Infinity VWD User Manual 12 Hardware Information Firmware Description 160 Optional Interface Boards 163 Electrical Connections 166 Serial Number Information ALL 167 Rear view of the module 168 Interfaces 169 Interfaces Overview 171 Setting the 8 bit Configuration Switch without On board LAN 175 Communication Settings for RS 232C 176 Special Settings 178 This chapter describes the detector in more detail on hardware and electronics E Agilent Technologies 159 12 Hardware Information Firmware Description 160 The firmware of the instrument consists of two independent sections anon instrument specific section called resident system aninstrument specific section called main system Resident System This resident section of the firmware is identical for all Agilent 1100 1200 1220 1260 1290 series modules Its properties 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 functions like run synchronization through APG remote error handling diagnostic functions
120. xternal equipment to the instrument make sure that you only use accessory units tested and approved according to the safety standards appropriate for the type of external equipment 116 Agilent 1260 Infinity VWD User Manual Maintenance 9 Overview of Maintenance The following pages describe maintenance simple repairs of the detector that can be carried out without opening the main cover Table 13 Simple Repairs Procedures Typical Frequency Notes Deuterium lamp If noise and or drift exceeds your application limits or A VWD test should be performed after exchange lamp does not ignite replacement Flow cell exchange If application requires a different flow cell type A VWD test should be performed after replacement Cleaning flow cell parts If leaking or if intensity drops due to contaminated flow A pressure tightness test should be cleaning or exchange cell windows done after repair Leak sensor drying If leak has occurred Check for leaks Leak handling system If broken or corroded Check for leaks replacement Agilent 1260 Infinity VWD User Manual 117 9 Maintenance Cleaning the Module To keep the module case clean use a soft cloth slightly dampened with water or a solution of water and mild detergent WARNING Liquid dripping into the electronic compartment of your module can cause shock hazard and damage the module gt Do not use an excessively damp cloth during cleaning Drain all solvent
121. y 189 defect on arrival 32 delivery checklist 33 detection type 25 27 detector error messages 90 Diagnostic software 80 diagnostic signals 76 test functions 99 dimensions 24 drift 25 27 initial 58 191 Index E electrical connections descriptions of 166 EMF early maintenance feedback 16 setting limits 17 using counters 16 entrance slit assembly 13 environment 23 error messages general 83 heater current missing 92 holmium oxide test failed 94 lamp current missing 90 lost CAN partner 85 remote timeout 84 error message ADC hardware error 96 error messages calibration failed 93 compensation sensor open 87 compensation sensor short 88 detector 90 fan failed 88 filter check failed 96 grating filter motor defective 94 ignition without cover 89 89 lamp ignition failed 91 lamp voltage missing 90 leak sensor open 86 leak sensor short 87 leak 86 shutdown 84 timeout 83 wavelength check failed 95 external contact cable 157 external contacts BCD board 163 192 F fan failed 88 features GLP 26 28 safety and maintenace 26 28 firmware description 160 main system 160 resident system 160 update tool 161 updates 131 160 131 upgade downgrade 131 upgrade downgrade 131 flow cell correction factors 73 exchange 122 high pressure parts 141 repairing 124 standard parts 135 types and data 25 27 frequency range 24 G general error messages 83 grating assembly 14 holmium oxide declaration of

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