Agilent Technologies 1260 User Manual

User Manual

Agilent 1260 Infinity Diode Array and Multiple Wavelength Detector

Agilent Technologies

Notices

No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.

Manual Part Number

G1315-90013

Edition

06/10

Printed in Germany

Agilent Technologies Hewlett-Packard-Strasse 8 76337 Waldbronn

Warranty

The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions. Further, to the maximum 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 particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate 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 accordance with the terms of such license.

Restricted Rights Legend

If software is for use in the performance of a U.S. Government prime contract or subcontract, 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 software” as defined in FAR 52.227-19 (June

1987) or any equivalent agency regulation or contract clause. Use, duplication or disclosure 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 performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.

WARNING

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 indicated conditions are fully understood and met.

For Research Use Only

Agilent 1260 Infinity DAD and MWD User Manual

In This Guide…

This manual covers the Agilent 1260 Infinity Diode Array and Multiple Wavelength Detector modules:

• G1315C - 1260 DAD VL+

• G1365C - 1260 MWD

• G1315D - 1260 DAD VL

• G1365D - 1260 MWD VL

1 Introduction

This chapter gives an introduction to the detector, instrument overview and internal connectors.

2 Site Requirements and Specifications

This chapter provides information on environmental requirements, physical and performance specifications.

In This Guide…

3 Installing the Module

This chapter gives information about the preferred stack setup for your system and the installation of your module.

4 LAN Configuration

This chapter provides information on connecting the detector to the Agilent ChemStation PC.

5 Using the Detector

This chapter provides information on how to set up the detector for an analysis and explains the basic settings.

6 How to optimize the Detector

This chapter provides information on how to optimize the detector.

Agilent 1260 Infinity DAD and MWD User Manual 3

In This Guide…

7 Troubleshooting and Diagnostics

This chapter gives an overview about the troubleshooting and diagnostic features and the different user interfaces.

8 Error Information

This chapter describes the meaning of error messages, and provides information on probable causes and suggested actions how to recover from error conditions.

9Test Functions

This chapter describes the detector’s built in test functions.

10 Maintenance

This chapter describes the maintenance of the detector.

11 Parts for Maintenance

This chapter provides information on parts for maintenance.

12 Identifying Cables

This chapter provides information on cables used with the 1200 series of HPLC modules.

13 Appendix

This chapter provides addition information on safety, legal and web.

4 Agilent 1260 Infinity DAD and MWD User Manual

Contents

1 Introduction 9

Introduction to the Detector 10 Optical System 11 Early Maintenance Feedback (EMF) 14 Instrument Layout 15 Electrical Connections 16 Interfaces 18 Setting the 8-bit Configuration Switch 24

2 Site Requirements and Specifications 33

Site Requirements 34 Physical Specifications 37 Performance Specifications 38

3 Installing the Module 43

Unpacking the Detector 44 Optimizing the Stack Configuration 46 Installing the Detector 50 Flow Connections to the Detector 53 Setting up the LAN access 56

4 LAN Configuration 57

What you have to do first 58 TCP/IP parameter configuration 59 Configuration Switch 60 Initialization mode selection 61 Link configuration selection 65 Automatic Configuration with BootP 66 Storing the settings permanently with Bootp 76 Manual Configuration 77

Agilent 1260 Infinity DAD and MWD User Manual 5

Contents

5 Using the Detector 83

Setting up an Analysis 84 Special Settings of the Detector 100 Special Setups with Multiple DAD-MWDs 114

6 How to optimize the Detector 115

Introduction 116 Optimization Overview 117 Optimizing for Sensitivity, Selectivity, Linearity and Dispersion 119 Optimizing Selectivity 129

7 Troubleshooting and Diagnostics 133

Overview of the Module’s Indicators and Test Functions 134 Status Indicators 135 User Interfaces 137 Agilent Lab Advisor Software 138

8 Error Information 139

What Are Error Messages 141 General Error Messages 142 Detector Error Messages 150

9 Test Functions 161

Self-test 162 Filter Test 164 Slit Test 166 Dark-Current Test 167 Intensity Test 170 Holmium Oxide Test 174 Spectral flatness test 177 ASTM Noise Test 178 Cell Test 179 Using the Built-in Test Chromatogram 181 Wavelength Verification and Recalibration 183 Test Chromatogram 184 Diagnosis Information on Agilent ChemStation 186 D/A Converter (DAC) Test 188

6 Agilent 1260 Infinity DAD and MWD User Manual

10 Maintenance 191

Introduction to Maintenance 192 Cautions and Warnings 193 Overview of Maintenance 195 Cleaning the Module 196 Exchanging a Lamp 197 Exchanging a Flow Cell 200 Maintenance of Standard, Semi-Micro or Micro Flow Cell 203 Maintenance of High Pressure Flow Cell 207 Replacing Capillaries on a Standard Flow Cell 209 Replacing Capillaries on a Semi-Micro and Micro Flow Cell 214 Nano Flow Cell - Replacing or Cleaning 218 Cleaning or Exchanging the Holmium Oxide Filter 223 Correcting Leaks 226 Replacing Leak Handling System Parts 227 Replacing the CompactFlash Card (G1315C/G1365C only) 228 Replacing the Module’s Firmware 229

11 Parts for Maintenance 231

Contents

Overview of Maintenance Parts 232 Standard Flow Cell 234 Semi-Micro Flow Cell Parts 236 Micro Flow Cell 238 Prep Flow Cell - SST 240 Prep Flow Cell - Quartz 242 Nano Flow Cells 244 High Pressure Flow Cell 248 Accessory Kits 250

12 Identifying Cables 253

Cable Overview 254 Analog Cables 256 Remote Cables 258 BCD Cables 261 CAN/LAN Cables 263 Agilent 1200 module to PC 264

Agilent 1260 Infinity DAD and MWD User Manual 7

Contents

13 Appendix 265

General Safety Information 266 The Waste Electrical and Electronic Equipment (WEEE) Directive (2002/96/EC) 269 Radio Interference 270 Sound Emission 271 UV-Radiation 272 Solvent Information 273 Declaration of Conformity for HOX2 Filter 275 Agilent Technologies on Internet 276

8 Agilent 1260 Infinity DAD and MWD User Manual

Agilent 1260 Infinity DAD and MWD User Manual

1 Introduction

Introduction to the Detector 10

Optical System 11

Early Maintenance Feedback (EMF) 14

Instrument Layout 15

Electrical Connections 16

Serial Number Information (ALL) 17 Rear view of the module 17

Interfaces 18

Interfaces Overview 20

Setting the 8-bit Configuration Switch 24

Communication Settings for RS-232C 28 Special Settings 30

This chapter gives an introduction to the detector, instrument overview and internal connectors.

Agilent Technologies

1 Introduction

Introduction to the Detector

The detector is designed for highest optical performance, GLP compliance and easy maintenance. It includes the following features:

• 80 Hz data acquisition rate for (ultra-) fast LC applications (requires

internal hard disk, G1315C and G1365C only),

• data recovery (DRC) feature provides data-never-lost insurance (requires

internal hard disk, G1315C and G1365C only),

• RFID tags for all flow cells and UV-lamps provides traceable information

about these assemblies,

• long-life deuterium with RFID tag and tungsten lamps for highest intensity

and lowest detection limit over a wavelength range of 190–950 nm,

• no loss in sensitivity for up to eight wavelengths simultaneous,

• programmable slit from 1–16 nm for complete optimization of sensitivity,

linearity and spectral resolution,

• optional flow-cell cartridges with RFID tag (standard 10 mm 13 µl,

semi-micro 6 mm 5 µl, micro 3 mm 2 µl, 80 nl, 500 nl, 10 mm, high pressure 10 mm 1.7 µl and prep-cells) are available and can be used depending on the application needs,

• easy front access to lamps and flow cell for fast replacement, and

• built-in holmium oxide filter for fast wavelength accuracy verification,

• built-in temperature control for improved baseline stability,

• additional diagnostic signals for temperature and lamp voltage monitoring,

For specifications, see “Performance Specifications” on page 38.

10 Agilent 1260 Infinity DAD and MWD User Manual

Optical System

The optical system of the detector is shown in Figure below. Its illumination source is a combination of a deuterium-arc-discharge lamp for the ultraviolet (UV) wavelength range and a tungsten lamp for the visible (VIS) and short-wave near-infrared (SWNIR) wavelength range. The image of the filament of the tungsten lamp is focused on the discharge aperture of the deuterium lamp by means of a special rear-access lamp design which allows both light sources to be optically combined and share a common axis to the source lens. The achromat (source lens) forms a single, focused beam of light through the flow cell. Each cell room and lamp are separated by a quartz window which can be cleaned or replaced. In the spectrograph, light is being dispersed onto the diode array by a holographic grating. This allows simultaneous access to all wavelength information.

8Zaahjeedgil^cYdl

Ijc\hiZcaVbe

Introduction

Optical System

8djea^c\aZch

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6X]gdbVihdjgXZaZch

=dab^jbdm^YZ[^aiZg

;adlXZaa

HeZXigdaZch

Ha^i

<gVi^c\

9^dYZVggVn

Figure 1 Optical System of the Detector

Agilent 1260 Infinity DAD and MWD User Manual 11

1 Introduction

Optical System

Lamps The light source for the UV-wavelength range is a deuterium lamp with a

shine-through aperture. As a result of plasma discharge in low-pressure deuterium gas, the lamp emits light over the 190 nm to approximately 800 nm wavelength range. The light source for the visible and SWNIR wavelength range is a low noise tungsten lamp. This lamp emits light over the wavelength range 470 – 950 nm.

Achromat

(Source Lens)

Holmium Oxide

Filter

Cell Support

Window

Flow Cell

Compartment

Spectrograph The spectrograph material is ceramic to reduce thermal effects to a minimum.

The achromat receives the light from both lamps and focuses it so that the beam passes through the flow cell.

The holmium oxide filter is electromechanically actuated. During the holmium filter test it moves into the light path.

The cell support window assembly separates the holmium filter area from the flow cell area.

The optical unit has a flow cell compartment for easy access to flow cells. A variety of optional flow cells can be inserted using the same quick, simple mounting system. The flow cell can be removed to check the optical and electronic performance of the detector without having influences from the flow cell.

The spectrograph consists of the spectrograph lens, the variable entrance slit, the grating and the photodiode array with front-end electronics. The spectrograph lens refocuses the light beam after it has passed through the flow cell. The sampling interval of the diode array is < 1 nm over the wavelength range 190 – 950 nm. Depending on the wavelength this varies from 1.0 to 1.25 diodes per nanometer (for example a diode every 0.8 to 1 nm).

For a small wavelength range, the small non-linearity could be neglected. With the wavelength range from 190 – 950 nm a new approach is required to achieve wavelength accuracy over the full range. Each spectrograph is calibrated individually. The calibration data is stored in the spectrograph on an EEPROM. Based on these data, the built-in processors calculate absorbance data with linear intervals (1.0, 2.0, …) between data points. This results in an excellent wavelength accuracy and instrument-to-instrument reproducibility.

Variable Entranc e

Slit System

12 Agilent 1260 Infinity DAD and MWD User Manual

The micro-slit system makes use of the mechanical properties of silicon combined with the precise structuring capabilities of bulk micro-machining. It combines the required optical functions — slit and shutter — in a simple and compact component. The slit width is directly controlled by the micro-processor of the instrument and can be set as method parameter.

Introduction

Optical System

Grating The combination of dispersion and spectral imaging is accomplished by using

a concave holographic grating. The grating separates the light beam into all its component wavelengths and reflects the light onto the photodiode array.

Diode Array The diode array is a series of 1024 individual photodiodes and control circuits

located on a ceramic carrier. With a wavelength range from 190 – 950 nm the sampling interval is < 1 nm.

Agilent 1260 Infinity DAD and MWD User Manual 13

1 Introduction

Early Maintenance Feedback (EMF)

Maintenance requires the exchange of components which are subject to wear or stress. Ideally, the frequency at which components are exchanged should be based on the intensity of usage of the module 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 Counters

EMF counters increment with use and can be assigned a maximum limit which

provides visual feedback in the user interface when the limit is exceeded. Some counters can be reset to zero after the required maintenance procedure.

Using the EMF Counters

The user-settable EMF limits for the EMF Counters enable the early maintenance feedback to be adapted to specific user requirements. The useful maintenance cycle is dependent on the requirements for use. Therefore, the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument.

Setting the EMF Limits

The setting of the EMF limits must be optimized over one or two maintenance cycles. Initially the default EMF limits should be set. When instrument performance indicates maintenance is necessary, take note of the values displayed by the EMF 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.

14 Agilent 1260 Infinity DAD and MWD User Manual

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 also helps to reduce or eliminate radio frequency emissions from the instrument itself.

Introduction

Instrument Layout

Agilent 1260 Infinity DAD and MWD User Manual 15

1 Introduction

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.

• Two independent analog outputs provide signals for integrators or data

handling.

• The REMOTE connector may be used in combination with other analytical

instruments from Agilent Technologies if you want to use features such as 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.

NOTE

16 Agilent 1260 Infinity DAD and MWD User Manual

Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.

Serial Number Information (ALL)

The serial number information on the instrument labels provide the following information:

CCXZZ00000 Format

CC Country of manufacturing (DE Germany)

X Alphabetic character A-Z (used by manufacturing)

ZZ Alpha-numeric code 0-9, A-Z, where each combination

unambiguously denotes a module (there can be more than one code for the same module)

00000 Serial number

Rear view of the module

Introduction

Electrical Connections

Figure 2 Rear View of Detector

Agilent 1260 Infinity DAD and MWD User Manual 17

1 Introduction

Interfaces

The Agilent 1200 Infinity Series modules provide the following interfaces:

Ta bl e 1 Agilent 1200 Infinity Series Interfaces

Module CAN LAN/BCD

(optional)

Pumps

G1310B Iso Pump G1311B Quat Pump G1311C Quat Pump VL G1312B Bin Pump G1312C Bin Pump VL 1376A Cap Pump G2226A Nano 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

Samplers

G1329B ALS G2260A Prep ALS

G1364B FC-PS G1364C FC-AS G1364D FCG1367E HiP ALS G1377A HiP micro ALS G2258A DL ALS

μS

2 Ye s N o Ye s 1 Ye s

2 Yes No Yes No Yes THERMOSTAT for

LAN (on-board)

RS-232 Analog APG

Remote

Special

slaves

G1330B

G1330B CAN-DC- OUT for CAN slaves

G4226A ALS 2 Yes No Yes No Yes

Detectors

G1314B VWD VL G1314C VWD VL+

G1314E/F VWD 2 No Yes Yes 1 Yes

2 Ye s N o Ye s 1 Ye s

18 Agilent 1260 Infinity DAD and MWD User Manual

Ta bl e 1 Agilent 1200 Infinity Series Interfaces

Introduction

Interfaces

Module CAN LAN/BCD

(optional)

G4212A/B DAD 2 No Yes Yes 1 Yes

G1315C DAD VL+ G1365C MWD G1315D DAD VL G1365D MWD VL

G1321B FLD G1362A RID

G4280A ELSD No No No Yes Yes Yes EXT Contact

Others

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

2 N o Ye s Ye s 2 Ye s

2 Ye s N o Ye s 1 Ye s

LAN (on-board)

RS-232 Analog APG

Remote

Special

AUTOZERO

slaves THERMOSTAT for G1330A/B (NOT USED)

NOTE

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

Agilent 1260 Infinity DAD and MWD User Manual 19

1 Introduction

Interfaces

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 G1369A/B 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 connected PC with the appropriate control software.

NOTE

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:

20 Agilent 1260 Infinity DAD and MWD User Manual

Ta bl e 2 RS-232C Connection Table

Pin Direction Function

1In DCD

2In RxD

3Out TxD

4 Out DTR

5Ground

6In DSR

7Out RTS

8In CTS

9In RI

Introduction

Interfaces

>chigjbZci

BVaZ ;ZbVaZ ;ZbVaZ BVaZ

Figure 3 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 DAD and MWD User Manual 21

1 Introduction

Interfaces

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 a ll connec t e d m odules. C o ntrol o f a nalysi s i s maintained by signa l r 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,

• input load is 2.2 kOhm against + 5.0 V, and

• output are open collector type, inputs/outputs (wired- or technique).

NOTE

22 Agilent 1260 Infinity DAD and MWD User Manual

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).

Introduction

Interfaces

Ta bl e 3 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, 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.

Agilent 1260 Infinity DAD and MWD User Manual 23

1 Introduction

Setting the 8-bit Configuration Switch

Setting the 8-bit Configuration Switch (with On-Board LAN)

The 8-bit configuration switch is located at the rear of the module. Switch settings provide configuration parameters for LAN, serial communication protocol and instrument specific initialization procedures.

All modules with on-board LAN, e.g. G1315/65C/D, G1314D/E, G4212A, G4220A:

• Default is ALL switches DOWN (best settings) - Bootp mode for LAN.

• For specific LAN modes switches 3-8 must be set as required.

• For boot/test modes switches 1+2 must be UP plus required mode.

Figure 4 Location of Configuration Switch

NOTE

24 Agilent 1260 Infinity DAD and MWD User Manual

To perform any LAN configuration, SW1 and SW2 must be set to OFF. For details on the LAN settings/configuration refer to chapter “LAN Configuration”.

Setting the 8-bit Configuration Switch

Ta bl e 4 8-bit Configuration Switch (with on-board LAN)

Mode Function

SW 1 SW 2 SW 3 SW 4 SW 5 SW 6 SW 7 SW 8

LAN 00 Link Configuration Init Mode Selection

Auto-negotiation 0 xxxxx

10 MBit, half-duplex 1 00xxx

10 MBit, full-duplex 1 0 1xxx

100 MBit, half-duplex 1 1 0 xxx

100 MBit, full-duplex 1 1 1 x x x

Bootp x x x 000

Bootp & Store x x x 001

Using Stored x x x 0 1 0

Using Default x x x 0 11

TEST 1 1 System NVRAM

Introduction

Boot Resident System 1 x

Revert to Default Data (Coldstart) x x x 1

Legend:

0 (switch down), 1 (switch up), x (any position)

NOTE

Agilent 1260 Infinity DAD and MWD User Manual 25

When selecting the mode TEST, the LAN settings are: Auto-Negotiation & Using Stored.

1 Introduction

Setting the 8-bit Configuration Switch

Setting the 8-bit Configuration Switch (without On-Board LAN)

The 8-bit configuration switch is located at the rear of the module.

Modules that do not have their own LAN interface (e.g. the TCC) can be controlled through the LAN interface of another module and a CAN connection to that module.

Figure 5 Configuration switch (settings depend on configured mode)

All modules without on-board LAN:

• default is ALL DIPS DOWN (best settings) - Bootp mode for LAN

• for boot/test modes DIPS 1+2 must be UP plus required mode

Switch settings provide configuration parameters for GPIB address, serial communication protocol and instrument specific initialization procedures.

NOTE

26 Agilent 1260 Infinity DAD and MWD User Manual

With the introduction of the Agilent 1260 Infinity, all GPIB interfaces have been removed. The preferred communication is LAN.

The following tables represent the configuration switch settings for the modules without on-board LAN only.

Introduction

Setting the 8-bit Configuration Switch

Ta bl e 5 8-bit Configuration Switch (without on-board LAN)

Mode Select12345678

NOTE

RS-232C 0 1 Baudrate Data

Bits

Reserved 1 0 Reserved

TEST/BOOT 1 1 RSVD SYS RSVD RSVD FC

Parity

The LAN settings are done on the LAN Interface Card G1369A/B. Refer to the documentation provided with the card.

Agilent 1260 Infinity DAD and MWD User Manual 27

1 Introduction

Setting the 8-bit Configuration Switch

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.

Ta bl e 6 Communication Settings for RS-232C Communication (without on-board LAN)

Mode

Select

RS-232C 0 1 Baudrate Data Bits Parity

12345 6 78

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.

Ta bl e 7 Baudrate Settings (without on-board LAN)

Switches Baud Rate Switches Baud Rate

345 345

0 0 0 9600 1 0 0 9600

0 0 1 1200 1 0 1 14400

0 1 0 2400 1 1 0 19200

0 1 1 4800 1 1 1 38400

Ta bl e 8 Data Bit Settings (without on-board LAN)

Switch 6 Data Word Size

0 7 Bit Communication

1 8 Bit Communication

28 Agilent 1260 Infinity DAD and MWD User Manual

Introduction

Setting the 8-bit Configuration Switch

Ta bl e 9 Parity Settings (without on-board LAN)

Switches Parity

0 0 No Parity

1 0 Odd Parity

11 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 DAD and MWD User Manual 29

1 Introduction

Setting the 8-bit Configuration Switch

Special Settings

The special settings are required for specific actions (normally in a service case).

NOTE

The tables include both settings for modules – with on-board LAN and without on-board LAN. They are identified as LAN and no LAN.

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).

Ta bl e 1 0 Boot Resident Settings (without on-board LAN)

Mode Select SW1 SW2 SW3 SW4 SW5 SW6 SW7 SW8

LAN TEST/BOOT11100000

No LAN TEST/BOOT11001000

30 Agilent 1260 Infinity DAD and MWD User Manual

Introduction

Setting the 8-bit Configuration Switch

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 diagnosis and repair log books which will not be erased.

➔ 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.

Ta bl e 1 1 Forced Cold Start Settings (without on-board LAN)

Mode Select SW1 SW2 SW3 SW4 SW5 SW6 SW7 SW8

LAN TEST/BOOT11000001

No LAN TEST/BOOT11001001

Agilent 1260 Infinity DAD and MWD User Manual 31

1 Introduction

Setting the 8-bit Configuration Switch

32 Agilent 1260 Infinity DAD and MWD User Manual

Agilent 1260 Infinity DAD and MWD User Manual

2 Site Requirements and Specifications

Site Requirements 34

Physical Specifications 37

Performance Specifications 38

Specifications 38 Specification Conditions 41

This chapter provides information on environmental requirements, physical and performance specifications.

Agilent Technologies

2 Site Requirements and Specifications

Site Requirements

A suitable environment is important to ensure optimal performance of the instrument.

Power Considerations

The module power supply has wide ranging capability. It accepts any line voltage in the range described in Table 12 on page 37. Consequently there is no voltage selector in the rear of the module. There are also no externally accessible fuses, because automatic electronic fuses are implemented in the power supply.

WARNING

CAUTION

Hazard of electrical shock or damage of your instrumentation

can result, if the devices are connected to a line voltage higher than specified.

➔ Connect your instrument to the specified line voltage only.

Module is partially energized when switched off, as long as the power cord is plugged in.

Repair work at the module can lead to personal injuries, e.g. electrical shock, when the cover is opened and the module is connected to power.

➔ Always unplug the power cable before opening the cover.

➔ Do not connect the power cable to the instrument while the covers are removed.

Unaccessable power plug.

In case of emergency it must be possible to disconnect the instrument from the power line at any time.

➔ Make sure the power connector of the instrument can be easily reached and

unplugged.

➔ Provide sufficient space behind the power socket of the instrument to unplug the

cable.

34 Agilent 1260 Infinity DAD and MWD User Manual

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.

Site Requirements and Specifications

Site Requirements

WARNING

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.

➔ Never operate your instrumentation from a power outlet that has no ground

connection.

➔ Never use a power cord other than the Agilent Technologies power cord designed

for your region.

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 Technologies to ensure

proper functionality and compliance with safety or EMC regulations.

Unintended use of supplied power cords

Using power cords for unintended purposes can lead to personal injury or damage of electronic equipment.

➔ Never use the power cords that Agilent Technologies supplies with this instrument

for any other equipment.

Agilent 1260 Infinity DAD and MWD User Manual 35

2 Site Requirements and Specifications

Site Requirements

Bench Space

The module dimensions and weight (see Table 12 on page 37) allow you to place the module on almost any desk or laboratory bench. It needs an additional 2.5 cm (1.0 inches) of space on either side and approximately 8 cm (3.1 inches) in the rear for air circulation and electric connections.

If the bench should carry an Agilent system, make sure that the bench is designed to bear the weight of all modules.

The module should be operated in a horizontal position.

Environment

Your detector will work within the specifications at ambient temperatures and relative humidity described in Table 12 on page 37.

ASTM drift tests require a temperature change below 2 °C/hour (3.6 °F/hour) over one hour period. Our published drift specification (refer also to

“Specifications” on page 38) 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.

NOTE

CAUTION

36 Agilent 1260 Infinity DAD and MWD User Manual

The module is designed to operate in a typical electromagnetic environment (EN61326-1) where RF transmitters, such as mobile phones, should not be used in close proximity.

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.

➔ 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.

Physical Specifications

Ta bl e 1 2 Physical Specifications

Type Specification Comments

Weight 11.5 kg (26 lbs)

Site Requirements and Specifications

Physical Specifications

Dimensions (height × width × depth)

Line voltage 100 – 240 VAC, ± 10% Wide-ranging capability

Line frequency 50 or 60 Hz, ± 5%

Power consumption 160 VA / 160 W / 546 BTU Maximum

Ambient operating temperature

Ambient non-operating temperature

Humidity < 95%, at 25–40 °C (77–104 °F) Non-condensing

Operating Altitude Up to 2000 m (6562 ft)

Non-operating altitude Up to 4600 m (15091 ft) For storing the module

Safety standards: IEC, CSA, ULInstallation Category II, Pollution Degree 2 For indoor use only.

140 x 345 x 435 mm (5.5 x 13.5 x 17 inches)

0–55 °C (32–131 °F)

-40–70 °C (-4–158 °F)

Agilent 1260 Infinity DAD and MWD User Manual 37

2 Site Requirements and Specifications

Performance Specifications

Specifications

Ta bl e 1 3 Performance Specifications G1315C/D and G1365C/D

Type Specification Comments

Detection type 1024-element photodiode array

Light source Deuterium and tungsten lamps The UV-lamp is equipped with RFID tag that

holds lamp typical information.

Data rate up to 80 Hz (G1315C/G1365C)

up to 20 Hz (G1315D/G1365D)

Wavelength range 190 – 950 nm

Short term noise (ASTM) Single and Multi-Wavelength

Drift

< ± 0.7·10

< 0.9·10

-5

AU at 254 and 750 nm

-3

AU/h at 254 nm

see "Specification Conditions" below

Linear absorbance range

Wavelength accuracy ± 1 nm Self-calibration with deuterium lines, verification

Wavelength bunching 1 – 400 nm Programmable in steps of 1 nm

Slit width 1, 2, 4 , 8, 16 nm Programmable slit

Diode width < 1 nm

> 2 AU (5 %) at 265 nm see "Specification Conditions" below

with holmium oxide filter

38 Agilent 1260 Infinity DAD and MWD User Manual

Site Requirements and Specifications

Ta bl e 1 3 Performance Specifications G1315C/D and G1365C/D

Type Specification Comments

Performance Specifications

Flow cells Standard: 13 µL volume, 10 mm cell path length

and 120 bar (1740 psi) pressure maximum Semi-micro: 5 µL volume, 6 mm cell path length and 120 bar (1740 psi) pressure maximum Micro: 2 µL volume, 3 mm cell path length, 120 bar (1740 psi) pressure maximum Semin-nano: 500 nL volume, 10 mm cell path length and 50 bar (725 psi) pressure maximum Nano: 80 nL volume, 10 mm cell path length and 50 bar (725 psi) pressure maximum High pressure: 1.7 µL volume, 6 mm cell path length and 400 bar (5800 psi) pressure maximum Prep SST: 3 mm cell path length and 120 bar (1740 psi) pressure maximum Prep Quartz:0.3 mm cell path length and 20 bar (290 psi) pressure maximum Prep Quartz: 0.06 mm cell path length and 20 bar (290 psi) pressure maximum

Time programmable Wavelength, polarity, peak width, lamp

bandwidth, autobalance, wavelength range, threshold, spectra storage mode

Spectral tools Data analysis software for spectra evaluation,

including spectral libraries and peak purity functions

See “Optimization Overview” on page 117 All flow cells are equipped with RFID tags that hold cell typical information.

Control and data evaluation

Local Control Agilent Instant Pilot (G4208A) For 1260 systems:

Analog outputs Recorder/integrator: 100 mV or 1 V, output

Agilent ChemStation for LC (32-bit) For 1260 systems:

• Revision B.04.02 DSP2 or above

For 1100/1200 systems:

• Revision B.01.03 or above (G1315C/G1365C)

• Revision B.01.03 SR-2 / B.02.01 SR-2 or

above (G1315D/G1365D)

• B.02.11 or above

For other systems:

• B.02.09 or above

range 0.001 – 2 AU, two outputs

Agilent 1260 Infinity DAD and MWD User Manual 39

2 Site Requirements and Specifications

Performance Specifications

Ta bl e 1 3 Performance Specifications G1315C/D and G1365C/D

Type Specification Comments

Communications Controller-area network (CAN), RS-232C, APG

Remote: ready, start, stop and shut-down signals, LAN

Safety and maintenance

GLP features RFID for electronics records of flow cell and UV

Housing All materials recyclable.

Others Electronic temperature control (ETC) for the

Extensive diagnostics, error detection and display (through control module and ChemStation), leak detection, safe leak handling, leak output signal for shutdown of pumping system. Low voltages in major maintenance areas.

lamp conditions (path length, volume, product number, serial number, test passed, usage) Early maintenance feedback (EMF) for continuous tracking of instrument usage in terms of lamp burn time with user-setable limits and feedback messages. Electronic records of maintenance and errors. Verification of wavelength accuracy with built-in holmium oxide filter.

complete optical unit

40 Agilent 1260 Infinity DAD and MWD User Manual

Specification Conditions

ASTM: “Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chromatography”.

Reference conditions: cell path length 10 mm, wavelength 254 and 750 nm with reference wavelength 360 nm/100 nm, slit width 4 nm, time constant 2 s (equal to response time 4 s), flow 1 mL/min LC-grade Methanol.

Linearity: Linearity is measured with caffeine at 265 nm/4 nm with slit width 4nm and TC 2s (or with RT 4s) with 10mm pathlength.

For environmental conditions refer to “Environment” on page 36

Site Requirements and Specifications

Performance Specifications

NOTE

The specifications are based on the standard RFID tag lamp (2140-0820) 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 (> two hours). ASTM measurements require that the detector should be turned on at least 24 h 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 DAD and MWD User Manual 41

2 Site Requirements and Specifications

Performance Specifications

42 Agilent 1260 Infinity DAD and MWD User Manual

Agilent 1260 Infinity DAD and MWD User Manual

3 Installing the Module

Unpacking the Detector 44

Damaged Packaging 44 Delivery Checklist 45

Optimizing the Stack Configuration 46

Two Stack Configuration 48

Installing the Detector 50

Flow Connections to the Detector 53

Setting up the LAN access 56

This chapter gives information about the preferred stack setup for your system and the installation of your module.

Agilent Technologies

3 Installing the Module

Unpacking the Detector

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.

CAUTION

"Defective on arrival" problems

If there are signs of damage, please do not attempt to install the module. Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged.

➔ Notify your Agilent sales and service office about the damage.

➔ An Agilent service representative will inspect the instrument at your site and

initiate appropriate actions.

44 Agilent 1260 Infinity DAD and MWD User Manual

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.

Ta bl e 1 4 Detector Checklist

Description Quantity

Detector 1

CompactFlash Card 1 (installed) G1315C/G1365C only

Power cable 1

Cross-over network cable 1

Twisted pair network cable 1

Flow cell As ordered

User Manual on Doumentation CD (part of the shipment - not

module specific)

Installing the Module

Unpacking the Detector

Accessory kit (p/n G1315-68755) 1

Agilent 1260 Infinity DAD and MWD User Manual 45

3 Installing the Module

Optimizing the Stack Configuration

If your detector is part of a complete Agilent 1200 Series system, you can ensure optimum performance by installing the following configuration. This configuration optimizes the system f low path, ensuring minimum delay volume.

HdakZciXVW^cZi

KVXjjbYZ\VhhZg

Ejbe

AdXVaJhZg>ciZg[VXZ

6jidhVbeaZg

8dajbcXdbeVgibZci

9ZiZXidg

Figure 6 Recommended Stack Configuration for 1260 (Front View)

46 Agilent 1260 Infinity DAD and MWD User Manual

GZbdiZXVWaZ

86C7jhXVWaZid adXVajhZg^ciZg[VXZ

86C7jhXVWaZ

Installing the Module

Optimizing the Stack Configuration

68edlZg

6cVad\YZiZXidg h^\cVa &dg'djiejih eZgYZiZXidg

A6CidA88]ZbHiVi^dc

adXVi^dcYZeZcYhdcYZiZXidg

Figure 7 Recommended Stack Configuration (Rear View)

Agilent 1260 Infinity DAD and MWD User Manual 47

3 Installing the Module

Optimizing the Stack Configuration

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 of this arrangement even without the autosampler thermostat. A slightly longer capillary is required between the pump and autosampler. (See Figure 8 on page 48 and Figure 9 on page 49).

>chiVciE^adi

9ZiZXidg

8dajbcXdbeVgibZci

6jidhVbeaZg

I]ZgbdhiVi[dgi]Z6AH dei^dcVa

HdakZciXVW^cZi

9Z\VhhZgdei^dcVa

Ejbe

Figure 8 Recommended Two Stack Configuration for 1260 (Front View)

48 Agilent 1260 Infinity DAD and MWD User Manual

A6CidXdcigdahd[ilVgZ

86C7jhXVWaZ id>chiVciE^adi

I]ZgbdXVWaZ dei^dcVa

GZbdiZXVWaZ

68EdlZg

Installing the Module

Optimizing the Stack Configuration

68EdlZg

86C7jhXVWaZ

68EdlZg

Figure 9 Recommended Two Stack Configuration for 1260 (Rear View)

Agilent 1260 Infinity DAD and MWD User Manual 49

3 Installing the Module

Installing the Detector

Parts required Description

Power cord

LAN cable (cross-over or twisted pair network cable)

All modules in the stack should have the latest firmware installed. If other revisions are required, check with the Agilent support for best match.

Hardware required Detector (as ordered)

Software required Appropriate control software or G4208A Instant Pilot (optional).

Preparations Locate bench space

Provide power connections

Unpack the module

WARNING

Module is partially energized when switched off, as long as the power cord is plugged in.

Repair work at the module can lead to personal injuries, e.g. shock hazard, when the cover is opened and the module is connected to power.

➔ Make sure that it is always possible to access the power plug.

➔ Remove the power cable from the instrument before opening the cover.

➔ Do not connect the power cable to the Instrument while the covers are removed.

NOTE

50 Agilent 1260 Infinity DAD and MWD User Manual

Before adding a G1315C/D and G1365C/D into an existing system assure that the existing modules have been updated to firmware revision A.06.02/B.01.02 or above. Otherwise the ChemStation “Performance Specifications” on page 38 will not recognize modules.

For G1315C and G1365C assure that the CompactFlash Card is installed in the rear of the module (required for operation).

Installing the Module

Installing the Detector

1 Note the MAC address of the LAN interface (rear of the module, under the

configuration switch, see Figure 10 on page 51). It’s required for “LAN

Configuration” on page 57.

2 Place the module in the stack or on the bench in a horizontal position.

3 Ensure the line power switch at the front of the module is OFF.

4 Connect the power cable to the power connector at the rear of the module.

EdlZg

Figure 10 Rear View of Detector

5 Connect the CAN cable to other Agilent 1200 Series modules.

6 Connect the LAN cable (e.g. from a Agilent ChemStation as controller) to

the detector's LAN connector.

NOTE

Agilent 1260 Infinity DAD and MWD User Manual 51

In multi-detector configurations the LAN of the G1315C/D and G1365C/D must be used due to its higher data load.

7 Connect the analog cable(s) (optional).

8 Connect the APG remote cable (optional) for non-Agilent 1200 Series

instruments.

3 Installing the Module

Installing the Detector

9 Turn on power by pushing the button at the lower left hand side of the

module. The status LED should be green.

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\gZZc$nZaadl$gZY

A^cZedlZghl^iX] l^i]\gZZca^\]i

Figure 11 Front View of Detector

NOTE

52 Agilent 1260 Infinity DAD and MWD User Manual

The module is turned on when the line power switch is pressed and the green indicator lamp is illuminated. The module is turned off when the line power switch is protruding and the green light is off.

The module was shipped with default configuration settings. To change these settings see

“Configuration Switch” on page 60.

Flow Connections to the Detector

Parts required # Description

G1315-68755 Accessory kit

Hardware required Other modules

Preparations Detector is installed in the LC system.

Installing the Module

Flow Connections to the Detector

WARNING

NOTE

Toxic, flammable and hazardous solvents, samples and reagents

The handling of solvents, samples and reagents can hold health and safety risks.

➔ 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.

➔ The amount of substances should be reduced to the minimal volume required for

the analysis.

➔ Do not operate the instrument in an explosive atmosphere.

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.

The detector should be operated with the front cover in place to protect the flow cell area against strong drafts from the outside and to cover the deuterium lamp.

Some types of the Agilent deuterium lamps show a light ring during operation. This is not harmful, refer to “UV-Radiation” on page 272.

Agilent 1260 Infinity DAD and MWD User Manual 53

3 Installing the Module

Flow Connections to the Detector

NOTE

Press the release buttons and remove the front cover to

gain access to the flow cell area.

3 Insert the flow cell. 4 Connect the flow cell capillaries to the capillary holder

The heat exchanger/capillary and the cell body can be fixed mirror symmetrically to have both capillaries routed to the bottom or to the top (depending on the routing of the capillaries to the column). For details see “Replacing Capillaries on a Standard Flow

Cell” on page 209.

2 Press the release button and open the flow cell door.

(top is inlet, bottom is outlet).

54 Agilent 1260 Infinity DAD and MWD User Manual

If another Agilent module is positioned on top of the detector, route the tubing assembly waste from the accessory kit behind the capillary holder and connect the top end to the other module’s waste outlet.

Iddi]ZgbdYjaZ

IdlVhiZ

Installing the Module

Flow Connections to the Detector

6 Connect the capillary from the column to the capillary

holder (top). Connect the teflon waste tubing to the flow cell outlet fitting (bottom) and the corrugated waste tubing to the leak outlet.

7 Remove the flow cell and establish a flow and observe for

leaks.

The installation of the detector is complete now.

8 Insert the flow cell, close the cover and replace the front

cover.

Agilent 1260 Infinity DAD and MWD User Manual 55

3 Installing the Module

Setting up the LAN access

Please follow the instructions in “LAN Configuration” on page 57

56 Agilent 1260 Infinity DAD and MWD User Manual

Agilent 1260 Infinity DAD and MWD User Manual

4 LAN Configuration

What you have to do first 58

TCP/IP parameter configuration 59

Configuration Switch 60

Initialization mode selection 61

Link configuration selection 65

Automatic Configuration with BootP 66

About Agilent BootP Service 66 How BootP Service Works 67 Situation: Cannot Establish LAN Communication 67 Installation of BootP Service 68 Two Methods to Determine the MAC Address 70 Assigning IP Addresses Using the Agilent BootP Service 71 Changing the IP Address of an Instrument Using the Agilent BootP

Service 74

Storing the settings permanently with Bootp 76

Manual Configuration 77

With Telnet 78 With the Instant Pilot (G4208A) 82

This chapter provides information on connecting the detector to the Agilent ChemStation PC.

Agilent Technologies

4 LAN Configuration

What you have to do first

The module has an on-board LAN communication interface.

1 Note the MAC (Media Access Control) address for further reference. The

MAC or hardware address of the LAN interfaces is a world wide unique identifier. No other network device will have the same hardware address. The MAC address can be found on a label at the rear of the module underneath the configuration switch (see Figure 13 on page 58).

Figure 12 MAC-Label

2 Connect the instrument's LAN interface (see Figure 13 on page 58) to

• the PC network card using a crossover network cable (point-to-point) or

• a hub or switch using a standard LAN cable.

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8djcignd[Dg^\^c

Figure 13 Location of LAN interface and MAC label

58 Agilent 1260 Infinity DAD and MWD User Manual

TCP/IP parameter configuration

To operate properly in a network environment, the LAN interface must be configured with valid TCP/IP network parameters. These parameters are:

• IP address

• Subnet Mask

• Default Gateway

The TCP/IP parameters can be configured by the following methods:

• by automatically requesting the parameters from a network-based BOOTP

Server (using the so-called Bootstrap Protocol)

• by manually setting the parameters using Telnet

• by manually setting the parameters using the Instant Pilot (G4208A)

The LAN interface differentiates between several initialization modes. The initialization mode (short form ‘init mode’) defines how to determine the active TCP/IP parameters after power-on. The parameters may be derived from a Bootp cycle, non-volatile memory or initialized with known default values. The initialization mode is selected by the configuration switch, see

Table 18 on page 65.

LAN Configuration

TCP/IP parameter configuration

Agilent 1260 Infinity DAD and MWD User Manual 59

4 LAN Configuration

Configuration Switch

The configuration switch can be accessed at the rear of the module.

Figure 14 Location of Configuration Switch

The module is shipped with all switches set to OFF, as shown above.

NOTE

60 Agilent 1260 Infinity DAD and MWD User Manual

To perform any LAN configuration, SW1 and SW2 must be set to OFF.

Ta bl e 1 5 Factory Default Settings

Initialization (‘Init’) Mode Bootp, all switches down. For details see “Initialization mode

selection” on page 61

Link Configuration speed and duplex mode determined by auto-negotiation, for

details see “Link configuration selection” on page 65

Initialization mode selection

The following initialization (init) modes are selectable:

Ta bl e 1 6 Initialization Mode Switches

SW 6 SW 7 SW 8 Init Mode

OFF OFF OFF Bootp

OFF OFF ON Bootp & Store

OFF ON OFF Using Stored

OFF ON ON Using Default

Bootp

When the initialization mode Bootp is selected, the module tries to download the parameters from a Bootp Server. The parameters obtained become the active parameters immediately. They are not stored to the non-volatile memory of the module. Therefore, the parameters are lost with the next power cycle of the module.

LAN Configuration

Initialization mode selection

7ddie HZgkZg

Figure 15 Bootp (Principle)

Agilent 1260 Infinity DAD and MWD User Manual 61

6Xi^kZ EVgVbZiZg

4 LAN Configuration

Initialization mode selection

Bootp & Store

When Bootp & Store is selected, the parameters obtained from a Bootp Server become the active parameters immediately. In addition, they are stored to the non-volatile memory of the module. Thus, after a power cycle they are still available. This enables a kind of bootp once configuration of the module.

Example: The user may not want to have a Bootp Server be active in his network all the time. But on the other side, he may not have any other configuration method than Bootp. In this case he starts the Bootp Server temporarily, powers on the module using the initialization mode Bootp & Store, waits for the Bootp cycle to be completed, closes the Bootp Server and powers off the module. Then he selects the initialization mode Using Stored and powers on the module again. From now on, he is able to establish the TCP/IP connection to the module with the parameters obtained in that single Bootp cycle.

NOTE

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Cdc"KdaVi^aZ

G6B

HidgZY EVgVbZiZg

6Xi^kZ EVgVbZiZg

Figure 16 Bootp & Store (Principle)

Use the initialization mode Bootp & Store carefully, because writing to the non-volatile memory takes time. Therefore, when the module shall obtain its parameters from a Bootp Server every time it is powered on, the recommended initialization mode is Bootp!

62 Agilent 1260 Infinity DAD and MWD User Manual

LAN Configuration

Initialization mode selection

Using Stored

When initialization mode Using Stored is selected, the parameters are taken from the non-volatile memory of the module. The TCP/IP connection will be established using these parameters. The parameters were configured previously by one of the described methods.

Cdc"KdaVi^aZ

G6B

6Xi^kZ

HidgZY

EVgVbZiZg

Figure 17 Using Stored (Principle)

EVgVbZiZg

Agilent 1260 Infinity DAD and MWD User Manual 63

4 LAN Configuration

Initialization mode selection

Using Default

When Using Default is selected, the factory default parameters are taken instead. These parameters enable a TCP/IP connection to the LAN interface without further configuration, see Table 17 on page 64.

NOTE

9Z[Vjai EVgVbZiZg

Figure 18 Using Default (Principle)

Using the default address in your local area network may result in network problems. Take care and change it to a valid address immediately.

Ta bl e 1 7 Using Default Parameters

IP address: 192.168.254.11

Subnet Mask: 255.255.255.0

Default Gateway not specified

Since the default IP address is a so-called local address, it will not be routed by any network device. Thus, the PC and the module must reside in the same subnet.

The user may open a Telnet session using the default IP address and change the parameters stored in the non-volatile memory of the module. He may then close the session, select the initialization mode Using Stored, power-on again and establish the TCP/IP connection using the new parameters.

6Xi^kZ EVgVbZiZg

When the module is wired to the PC directly (e.g. using a cross-over cable or a local hub), separated from the local area network, the user may simply keep the default parameters to establish the TCP/IP connection.

NOTE

64 Agilent 1260 Infinity DAD and MWD User Manual

In the Using Default mode, the parameters stored in the memory of the module are not cleared automatically. If not changed by the user, they are still available, when switching back to the mode Using Stored.

Link configuration selection

The LAN interface supports 10 or 100 Mbps operation in full- or half-duplex modes. In most cases, full-duplex is supported when the connecting network device - such as a network switch or hub - supports IEEE 802.3u auto-negotiation specifications.

When connecting to network devices that do not support auto-negotiation, the LAN interface will configure itself for 10- or 100-Mbps half-duplex operation.

For example, when connected to a non-negotiating 10-Mbps hub, the LAN interface will be automatically set to operate at 10-Mbps half-duplex.

If the module is not able to connect to the network through auto-negotiation, you can manually set the link operating mode using link configuration switches on the module.

Ta bl e 1 8 Link Configuration Switches

SW 3 SW 4 SW 5 Link Configuration

LAN Configuration

Link configuration selection

OFF - - speed and duplex mode determined by

auto-negotiation

ON OFF OFF manually set to 10 Mbps, half-duplex

ON OFF ON manually set to 10 Mbps, full-duplex

ON ON OFF manually set to 100 Mbps, half-duplex

ON ON ON manually set to 100 Mbps, full-duplex

Agilent 1260 Infinity DAD and MWD User Manual 65

4 LAN Configuration

Automatic Configuration with BootP

NOTE

All examples shown in this chapter will not work in your environment. You need your own IP-, Subnet-Mask- and Gateway addresses.

Assure that the detector configuration switch is set properly. The setting should be either BootP or BootP & Store, see Ta b l e 1 6 on page 61.

Assure that the detector connected to the network is powered off.

If the Agilent BootP Service program is not already installed on your PC, then install it from your Agilent ChemStation DVD, located in folder BootP.

About Agilent BootP Service

The Agilent BootP Service is used to assign the LAN Interface with an IP address.

The Agilent BootP Service is provided on the ChemStation DVD. The Agilent BootP Service is installed on a server or PC on the LAN to provide central administration of IP addresses for Agilent instruments on a LAN. The BootP service must be running TCP/IP network protocol and cannot run a DHCP server.

66 Agilent 1260 Infinity DAD and MWD User Manual

Automatic Configuration with BootP

How BootP Service Works

When an instrument is powered on, an LAN Interface in the instrument broadcasts a request for an IP address or host name and provides its hardware MAC address as an identifier. The Agilent BootP Service answers this request and passes a previously defined IP address and host name associated with the hardware MAC address to the requesting instrument.

The instrument receives its IP address and host name and maintains the IP address as long as it is powered on. Powering down the instrument causes it to lose its IP address, so the Agilent BootP Service must be running every time the instrument powers up. If the Agilent BootP Service runs in the background, the instrument will receive its IP address on power-up.

The Agilent LAN Interface can be set to store the IP address and will not lose the IP address if power cycled.

Situation: Cannot Establish LAN Communication

If a LAN communication with BootP service cannot be established, check the following on the PC:

• Is the BootP service started? During installation of BootP, the service is not

started automatically.

• Does the Firewall block the BootP service? Add the BootP service as an

exception.

• Is the LAN Interface using the BootP-mode instead of "Using Stored" or

"Using Default" modes?

LAN Configuration

Agilent 1260 Infinity DAD and MWD User Manual 67

4 LAN Configuration

Automatic Configuration with BootP

Installation of BootP Service

Before installing and configuring the Agilent BootP Service, be sure to have the IP addresses of the computer and instruments on hand.

1 Log on as Administrator or other user with Administrator privileges.

2 Close all Windows programs.

3 Insert the Agilent ChemStation software DVD into the drive. If the setup

program starts automatically, click Cancel to stop it.

4 Open Windows Explorer.

5 Go to the BootP directory on the Agilent ChemStation DVD and double-click

BootPPackage.msi.

6 If necessary, click the Agilent BootP Service... icon in the task bar.

7 The Welcome screen of the Agilent BootP Service Setup Wizard appears. Click

Next.

8 The End-User License Agreement screen appears. Read the terms, indicate

acceptance, then click Next.

9 The Destination Folder selection screen appears. Install BootP to the default

folder or click Browse to choose another location. Click Next.

The default location for installation is:

C:\Program Files\Agilent\BootPService\

10 Click Install to begin installation.

68 Agilent 1260 Infinity DAD and MWD User Manual

LAN Configuration

Automatic Configuration with BootP

11 Files load; when finished, the BootP Settings screen appears.

Figure 19 BootP Settings screen

12 In the Default Settings part of the screen, if known, you can enter the subnet

mask and gateway.

Defaults can be used:

• The default subnet mask is 255.255.255.0.

• The default gateway is 10.1.1.101.

13 On the BootP Settings screen, click OK. The Agilent BootP Service Setup screen

indicates completion.

14 Click Finish to exit the Agilent BootP Service Setup screen.

15 Remove the DVD from the drive.

This completes installation.

16 Start the BootP service. On the Windows® desktop, select Start > Control

Panel > Services. Select the Agilent BootP Service and click Start.

Agilent 1260 Infinity DAD and MWD User Manual 69

4 LAN Configuration

Automatic Configuration with BootP

Two Methods to Determine the MAC Address

Enabling logging to discover the MAC address using BootP

If you want to see the MAC address, select the Do you want to log BootP requests? check box.

1 Open BootP Settings from Start > All Programs > Agilent BootP Service >

EditBootPSettings.

2 In BootP Settings... check Do you want to log BootP requests? to enable logging.

Figure 20 Enable BootP logging

The log file is located in

C:\Documents and Settings\All Users\Application Data\Agilent\BootP\LogFile

It contains a MAC address entry for each device that requests configuration information from BootP.

3 Click OK to save the values or Cancel to discard them. The editing ends.

4 After each modification of the BootP settings (i.e. EditBootPSettings) a stop

or start of the BootP service is required for the BootP service to accept changes. See “Stopping the Agilent BootP Service” on page 74 or “Restarting

the Agilent BootP Service” on page 75.

5 Uncheck the Do you want to log BootP requests? box after configuring

instruments; otherwise, the log file will quickly fill up disk space.

Determining the MAC address directly from the LAN Interface card label

1 Turn off the instrument.

2 Read the MAC address from the label and record it.

The MAC address is printed on a label on the rear of the module. It is the number below the barcode and after the colon (:) and usually begins with the letters AD, see Figure 12 on page 58 and Figure 13 on page 58.

3 Turn on the instrument.

70 Agilent 1260 Infinity DAD and MWD User Manual

LAN Configuration

Automatic Configuration with BootP

Assigning IP Addresses Using the Agilent BootP Service

The Agilent BootP Service assigns the Hardware MAC address of the instrument to an IP address.

Determining the MAC address of the instrument using BootP Service

1 Power cycle the Instrument.

2 After the instrument completes self-test, open the log file of the BootP

Service using Notepad.

• The default location for the logfile is C:\Documents and Settings\All Users\ Application Data\Agilent\BootP\LogFile.

• The logfile will not be updated if it is open.

The contents will be similar to the following:

02/25/10 15:30:49 PM

Status: BootP Request received at outermost layer

Status: BootP Request received from hardware address: 0010835675AC

Error: Hardware address not found in BootPTAB: 0010835675AC

Status: BootP Request finished processing at outermost layer

3 Record the hardware (MAC) address (for example, 0010835675AC).

4 The Error means the MAC address has not been assigned an IP address and

the Tab File does not have this entry. The MAC address is saved to the Tab File when an IP address is assigned.

5 Close the log file before turning on another instrument.

6 Uncheck the Do you want to log BootP requests? box after configuring

instruments to avoid having the logfile use up excessive disk space.

Agilent 1260 Infinity DAD and MWD User Manual 71

4 LAN Configuration

Automatic Configuration with BootP

Adding each instrument to the network using BootP

1 Follow Start > All Programs > Agilent BootP Service and select Edit BootP

Settings. The BootP Settings screen appears.

2 Uncheck the Do you want to log BootP requests? once all instruments have been

added.

The Do you want to log BootP requests? box must be unchecked when you have finished configuring instruments; otherwise, the log file will quickly fill up disk space.

3 Click Edit BootP Addresses... The Edit BootP Addresses screen appears.

4 Click Add... The Add BootP Entry screen appears.

Figure 21 Enable BootP logging

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LAN Configuration

Automatic Configuration with BootP

5 Make these entries for the instrument:

• MAC address

• Host name, Enter a Hostname of your choice.

The Host Name must begin with "alpha" characters (i.e. LC1260)

• IP address

• Comment (optional)

• Subnet mask

• Gateway address (optional)

The configuration information entered is saved in the Tab File.

6 Click OK.

7 Leave Edit BootP Addresses by pressing Close.

8 Exit BootP Settings by pressing OK.

9 After each modification of the BootP settings (i.e. EditBootPSettings) a stop

or start of the BootP service is required for the BootP service to accept changes. See “Stopping the Agilent BootP Service” on page 74 or “Restarting

the Agilent BootP Service” on page 75.

10 Power cycle the Instrument.

If you changed the IP address, power cycle the instrument for the changes to take effect.

11 Use the PING utility to verify connectivity by opening a command window

and typing:

Ping 10.1.1.101 for example.

The Tab File is located at

C:\Documents and Settings\All Users\Application Data\Agilent\BootP\TabFile

Agilent 1260 Infinity DAD and MWD User Manual 73

4 LAN Configuration

Automatic Configuration with BootP

Changing the IP Address of an Instrument Using the Agilent BootP Service

Agilent BootP Service starts automatically when your PC reboots. To change Agilent BootP Service settings, you must stop the service, make the changes, and then restart the service.

Stopping the Agilent BootP Service

1 From the Windows control panel, select Administrative Tools > Services. The

Services screen appears.

Figure 22 Windows Services screen

2 Right-click Agilent BootP Service.

3 Select Stop.

4 Close the Services and Administrative Tools screen.

74 Agilent 1260 Infinity DAD and MWD User Manual

LAN Configuration

Automatic Configuration with BootP

Editing the IP address and other parameters in EditBootPSettings

1 Select Start > All Programs > Agilent BootP Service and select Edit BootP Settings.

The BootP Settings screen appears.

2 When the BootP Settings screen is first opened, it shows the default settings

from installation.

3 Press Edit BootP Addresses… to edit the Tab File.

Figure 23 Edit BootP Adresses screen

4 In the Edit BootP Addresses... screen press Add... to create a new entry or

select an existing line from the table and press Modify... or Delete to change the IP address, comment, subnet mask, for example, in the Tab File.

If you change the IP address, it will be necessary to power cycle the instrument for the changes to take effect.

5 Leave Edit BootP Addresses... by pressing Close.

6 Exit BootP Settings by pressing OK.

Restarting the Agilent BootP Service

1 In the Windows control panel, select Administrative Tools > Services. The

Services screen appears, see Figure 22 on page 74.

2 Right-click Agilent BootP Service and select Start.

3 Close the Services and Administrative Tools screens.

Agilent 1260 Infinity DAD and MWD User Manual 75

4 LAN Configuration

Storing the settings permanently with Bootp

If you want to change parameters of the module using the Bootp follow the instructions below.

1 Turn off the module.

2 Change the module's settings of the Configuration Switch to “Bootp &

Store” mode, see Table 16 on page 61.

3 Start the Agilent Bootp Service and open its window.

4 If required, modify the parameters for the module according to your needs

using the existing configuration.

5 Press OK to exit the Bootp Manager.

6 Now turn on the module and view the Bootp Server window. After some

time the Agilent Bootp Service will display the request from the LAN interface. The parameters are now stored permanently in the non-volatile memory of the module.

7 Close the Agilent Bootp Service and turn off the module.

8 Change the settings of the module’s Configuration Switch to “Using Stored”

mode, see Table 16 on page 61.

9 Power cycle the module. The module can be accessed now via LAN without

the Agilent Bootp Service.

76 Agilent 1260 Infinity DAD and MWD User Manual

Manual Configuration

Manual configuration only alters the set of parameters stored in the non-volatile memory of the module. It never affects the currently active parameters. Therefore, manual configuration can be done at any time. A power cycle is mandatory to make the stored parameters become the active parameters, given that the initialization mode selection switches are allowing it.

I:AC:I

HZhh^dc

Manual Configuration

Cdc"KdaVi^aZ

G6B

HidgZY

EVgVbZiZg

LAN Configuration

8dcigda BdYjaZ

Figure 24 Manual Configuration (Principle)

Agilent 1260 Infinity DAD and MWD User Manual 77

4 LAN Configuration

Manual Configuration

With Telnet

Whenever a TCP/IP connection to the module is possible (TCP/IP parameters set by any method), the parameters may be altered by opening a Telnet session.

1 Open the system (DOS) prompt window by clicking on Windows START

2 Type the following at the system (DOS) prompt:

button and select “Run...”. Type “cmd” and press OK.

• c:\>telnet <IP address> or

• c:\>telnet <host name>

Figure 25 Telnet - Starting a session

where <IP address> may be the assigned address from a Bootp cycle, a configuration session with the Handheld Controller, or the default IP address (see “Configuration Switch” on page 60).

When the connection was established successfully, the module responds with the following:

Figure 26 A connection to the module is made

78 Agilent 1260 Infinity DAD and MWD User Manual

LAN Configuration

Manual Configuration

3 Type

? and press enter to see the available commands.

Figure 27 Telnet Commands

Ta bl e 1 9 Telnet Commands

Value Description

? displays syntax and descriptions of commands

/ displays current LAN settings

ip <x.x.x.x> sets new ip address

sm <x.x.x.x> sets new subnet mask

gw <x.x.x.x> sets new default gateway

exit exits shell and saves all changes

4 To change a parameter follows the style:

• parameter value, for example:

ip 134.40.27.230

Then press [Enter], where parameter refers to the configuration parameter you are defining, and value refers to the definitions you are assigning to that parameter. Each parameter entry is followed by a carriage return.

Agilent 1260 Infinity DAD and MWD User Manual 79

4 LAN Configuration

Manual Configuration

5 Use the “/” and press Enter to list the current settings.

Figure 28 Telnet - Current settings in "Using Stored" mode

6 Change the IP address (in this example 134.40.27.99) and type “/” to list

current settings.

information about the LAN interface MAC address, initialization mode Initialization mode is Using Stored active TCP/IP settings TCP/IP status - here ready connected to PC with controller software (e.g. Agilent ChemStation), here not connected

change of IP setting to Initialization mode is Using Stored active TCP/IP settings stored TCP/IP settings in non-volatile memory

connected to PC with controller software (e.g. Agilent ChemStation), here not connected

Figure 29 Telnet - Change IP settings

80 Agilent 1260 Infinity DAD and MWD User Manual

LAN Configuration

Manual Configuration

7 When you have finished typing the configuration parameters, type

exit and press Enter to exit with storing parameters.

Figure 30 Closing the Telnet Session

NOTE

If the Initialization Mode Switch is changed now to “Using Stored” mode, the instrument will take the stored settings when the module is re-booted. In the example above it would be 134.40.27.99.

Agilent 1260 Infinity DAD and MWD User Manual 81

4 LAN Configuration

Manual Configuration

With the Instant Pilot (G4208A)

To configure the TCP/IP parameters before connecting the module to the network, the Instant Pilot (G4208A) can be used.

1 From the Welcome screen press the More button.

2 Select Configure.

3 Press the DAD button.

4 Scroll down to the LAN settings.

Figure 31 Instant Pilot - LAN Configuration

5 Press the Edit button (only visible if not in Edit mode), perform the required

changes and press the Done button.

6 Leave the screen by clicking Exit.

82 Agilent 1260 Infinity DAD and MWD User Manual

Agilent 1260 Infinity DAD and MWD User Manual

5 Using the Detector

Setting up an Analysis 84

Before Using the System 84 Requirements and Conditions 86 Optimization of the System 89 Preparing the HPLC System 90 Running the Sample and Verifying the Results 99

Special Settings of the Detector 100

Control Settings 100 Configuration Settings 101 Online Spectra (DAD only) 102 Run Recovery Settings 103 Automated Run Recovery in case of temporary communication

failures 104 Manual Run Recovery in case of permanent communication

failures 106 Analog Output Settings 107 Spectrum Settings (DAD only) 108 Peakwidth Settings 110 Slit Settings 112 Margin for Negative Absorbance Settings 113 Optimizing the Detector 113

Special Setups with Multiple DAD-MWDs 114

Two detectors of same type (e.g. G1315C/D and G1315C/D) 114 Two detectors of similar type (e.g. G1315C/D and G1315A/B) 114

This chapter provides information on how to set up the detector for an analysis and explains the basic settings.

Agilent Technologies

5 Using the Detector

Setting up an Analysis

This chapter may be used to

• Prepare the system,

• Get to know the set up of an HPLC analysis and

• Use it as an instrument check to demonstrate that all modules of the system

are correctly installed and connected. It is not a test of the instrument performance.

• Learn about special settings

Before Using the System

Solvent Information

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

Priming and Purging the System

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

84 Agilent 1260 Infinity DAD and MWD User Manual

Ta bl e 2 0 Choice of Priming Solvents for Different Purposes

Activity Solvent Comments

Using the Detector

Setting up an Analysis

After an installation

When switching between reverse phase and normal phase (both times)

After an installation Ethanol or Methanol Alternative to Isopropanol (second

Cleaning the system when using buffers

After a solvent change

After the installation of normal phase seals (P/N 0905-1420)

NOTE

The pump should never be used for priming empty tubings (never let the pump run dry). Use a syringe to draw enough solvent to completely fill the tubings up to the pump inlet before

Isopropanol

Bidistilled water

Hexane + 5% Isopropanol Good wetting properties

Best solvent to flush air out of the system

choice) if no Isopropanol is available

Best solvent to re-dissolve buffer crystals

you continue priming 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 Set flow to required value of your application and close the purge valve.

Pump for approximately 10 minutes before starting your application.

Agilent 1260 Infinity DAD and MWD User Manual 85

5 Using the Detector

Setting up an Analysis

Requirements and Conditions

Parts and Material required

Table 21 on page 86 lists the parts and material you need for the set up of the

analysis. Some of these are optional (not required for the basic system).

Ta bl e 2 1 Parts and Material required

Agilent 1260 Infinity system

Column: Zorbax Eclipse XDB C18, 150 mm x 4.6 mm, 5 µm (p/n 993967-906)

Standard: Agilent isocratic checkout sample (p/n 01080-68704). This 0.5 mL

Pump (plus degassing)

Autosampler

Detector, standard flow cell installed

• Agilent ChemStation or

• Instant Pilot G4208 (optional for basic operation) or

with with the appropriate revisions, see “Performance Specifications” on page 38.

System should be correctly set up for LAN communication with the Data System

ampoule contains 0.15 wt.% dimethylphthalate, 0.15 wt.% diethylphthalate,

0.01 wt.% biphenyl, 0.03 wt.% o-terphenyl in methanol.

86 Agilent 1260 Infinity DAD and MWD User Manual

Using the Detector

Setting up an Analysis

Conditions

A single injection of the isocratic test standard is made under the conditions given in Table 22 on page 87:

Ta bl e 2 2 Conditions

Flow 1.5 ml/minute

Stoptime 8 minutes

Solvent 100% (30% water/70% Acetonitrile)

Temperature Ambient

Wavelength sample 254 nm (4 nm bandwidth) reference 360 nm (100 nm bandwidth)

Injection Volume 1 µl

Agilent 1260 Infinity DAD and MWD User Manual 87

5 Using the Detector

Setting up an Analysis

Typical Chromatogram

A typical chromatogram for this analysis is shown in Figure 32 on page 88. The exact profile of the chromatogram will depend on the chromatographic conditions. Variations in solvent quality, column packing, standard concentration and column temperature will all have a potential effect on peak retention and response.

Figure 32 Typical Chromatogram with UV-detector

88 Agilent 1260 Infinity DAD and MWD User Manual

Optimization of the System

The settings used for this analysis are specific for this purpose. For other applications the system can be optimized in various ways. Please refer to the section “Optimizing the Detector” on page 113.

Using the Detector

Setting up an Analysis

Agilent 1260 Infinity DAD and MWD User Manual 89

5 Using the Detector

Setting up an Analysis

Preparing the HPLC System

1 Turn on the Agilent ChemStation PC and the monitor.

2 Turn on the HPLC modules.

3 Start the Agilent ChemStation software. If the pump, autosampler,

HnhiZbhiVijh

thermostatted column compartment and detector are found, the ChemStation screen should look like shown in Figure below.

The System status is red (Not Ready).

Dc"a^cZeadil^cYdl

YZiV^ahl^cYdl

Figure 33 Initial ChemStation screen (Method and Run Control)

90 Agilent 1260 Infinity DAD and MWD User Manual

Using the Detector

Setting up an Analysis

4 Turn on the detector lamp, pump and autosampler by clicking the System On

button or the buttons below the module icons on the graphical user interface (GUI). After some time, the pump, thermostatted column compartment and detector module will turn to green.

Figure 34 Turning on the HPLC Module

Agilent 1260 Infinity DAD and MWD User Manual 91

5 Using the Detector

Setting up an Analysis

5 Purge the pump. For more information see “Priming and Purging the

6 Allow the detector to warm up at least 60 minutes to provide a stable

System” on page 84.

baseline (see example in Figure 35 on page 92 and Table 23 on page 92).

NOTE

For reproducible chromatography, the detector and lamp should be on for at least one hour. Otherwise the detector baseline may still drift (depending on the environment). See also section Wander/Drift Problems Due to Temperature Changesin the Service Manual..

Figure 35 Stabilization of Baseline (both lamps turned on at the same time)

Ta bl e 2 3 Baseline drift after lamp turn on (example from Figure above)

Time [minutes] Drift [mAU/hr]

17 - 20 2.6

27 - 30 0.8

37 - 40 0.4

47 - 50 0.2

57 - 60 < 0.2

92 Agilent 1260 Infinity DAD and MWD User Manual

Using the Detector

Setting up an Analysis

7 For the isocratic pump, fill the solvent bottle with the mixture of

HPLC-grade bi-distilled water (30 %) and acetonitrile (70 %). For binaryand quaternary pumps you can use separate bottles.

8 Click on the Load Method button and select DEF_LC.M and press OK.

Alternative double-click on the method in the method window. The default LC method parameters are transferred into the modules.

Figure 36 Loading Default LC Method

Agilent 1260 Infinity DAD and MWD User Manual 93

5 Using the Detector

Setting up an Analysis

9 Click on the module icons (see Figure below) and open the Setup of these

modules. Figure on page 95 shows the detector settings (do not change the detector parameters at this time).

Figure 37 Open the module menu

94 Agilent 1260 Infinity DAD and MWD User Manual

Using the Detector

Setting up an Analysis

10 Enter the pump parameters mentioned under Table 22 on page 87.

• up to 8 signals (A to H) with individual wavelength

settings can be selected.

• spectrum settings, “Spectrum Settings (DAD only)” on page 108

• stop and post time can be set (if required)

• depending on the application, the lamps can be

selected (one or both).

• peak width depends on the peaks in the chromatogram,

“Peakwidth Settings” on page 110

• autobalance to zero absorbance (on the analog output plus offset) at begin and/or end of run.

• mechanical slit width can be changed for further optimization, “Slit Settings” on page 112

• margin for negative absorbance, “Margin for Negative

Absorbance Settings” on page 113

• Under More additional diagnostic signals can be added for troubleshooting purpose, see section “Diagnostic Signals“ in the Service Manual.

• time table for programmable actions during the run. NOTE: The Agilent G1315C/D and G1365C/D time table can contain a maximum of 60 rows.

11 Pump the water/acetonitrile (30/70 %) mobile phase through the column for

10 minutes for equilibration.

Agilent 1260 Infinity DAD and MWD User Manual 95

5 Using the Detector

Setting up an Analysis

12 Click the button and select Change... to open the Signal Plot information.

Select the Pump: Pressure and the DAD A: Signal 254,4 as signals. Change the Y-range for the DAD to 1 mAU and the offset to 20% and the pressure offset to 50%. The X-axis range should be 15 minutes. Press OK to exit this screen.

Figure 38 Edit Signal Plot Window

The Online Plot (Figure 39 on page 97) 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.

96 Agilent 1260 Infinity DAD and MWD User Manual

Using the Detector

Setting up an Analysis

EjbeegZhhjgZh^\cVa

969VWhdgWVcXZh^\cVa

Figure 39 Online Plot Window

13 If both baselines are stable, set the Y-range for the detector signal to

100 mAU.

NOTE

Agilent 1260 Infinity DAD and MWD User Manual 97

If you start with a new UV-lamp for the first time, the lamp may show initial drift for some time (burn-in effect).

5 Using the Detector

Setting up an Analysis

14 Select the menu item RunControl -> Sample Info and enter information about

this application (see figure below). Press OK to leave this screen.

Figure 40 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).

98 Agilent 1260 Infinity DAD and MWD User Manual

Running the Sample and Verifying the Results

1 To start a run select the menu item RunControl -> Run Method.

2 This will start the modules and the online plot on the Agilent ChemStation

will show the resulting chromatogram.

Using the Detector

Setting up an Analysis

Figure 41 Chromatogram with Isocratic Test Sample

NOTE

Agilent 1260 Infinity DAD and MWD User Manual 99

Information about using the Data Analysis functions can be obtained from the Using your ChemStation manual supplied with your system.

5 Using the Detector

Special Settings of the Detector

In this chapter special settings of the G1315C/D and G1365C/D are described (based on the Agilent ChemStation B.02.01).

Control Settings

•Lamps: turn on and off of UV- and Vis lamp

•At Power On: automatic lamp-on at power on.

• Error Method: take error method or current method (in

case of an error)

• Analog Output Range: can be set to either 100 mV or 1 V full scale, “Analog Output Settings” on page 107

• Automatic Turn On: lamps can be programmed (detector must be on for this).

•Help: online help.

Figure 42 Detector control settings

100 Agilent 1260 Infinity DAD and MWD User Manual

Agilent Technologies 1260 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

In This Guide…

Introduction to the Detector

Optical System

Early Maintenance Feedback (EMF)

Instrument Layout

Electrical Connections

Serial Number Information (ALL)

Rear view of the module

Interfaces

Interfaces Overview

Setting the 8-bit Configuration Switch

Setting the 8-bit Configuration Switch (with On-Board LAN)

Setting the 8-bit Configuration Switch (without On-Board LAN)

Communication Settings for RS-232C

Special Settings

Site Requirements

Power Considerations

Power Cords

Bench Space

Environment

Physical Specifications

Performance Specifications

Specifications

Specification Conditions

Unpacking the Detector

Damaged Packaging

Delivery Checklist

Optimizing the Stack Configuration

Two Stack Configuration

Installing the Detector

Flow Connections to the Detector

Setting up the LAN access

What you have to do first

TCP/IP parameter configuration

Configuration Switch

Initialization mode selection

Link configuration selection

Automatic Configuration with BootP

About Agilent BootP Service

How BootP Service Works

Situation: Cannot Establish LAN Communication

Installation of BootP Service

Two Methods to Determine the MAC Address

Assigning IP Addresses Using the Agilent BootP Service

Changing the IP Address of an Instrument Using the Agilent BootP Service

Storing the settings permanently with Bootp

Manual Configuration

With Telnet

With the Instant Pilot (G4208A)

Setting up an Analysis

Before Using the System

Requirements and Conditions

Optimization of the System

Preparing the HPLC System

Running the Sample and Verifying the Results

Special Settings of the Detector

Control Settings