Agilent Technologies 1260 Infinity Manuel utilisateur

Agilent Technologies

Agilent 1260 Infinity

Purification Solution

Method Developer's

Quick Start Guide

Purification Solution - Developer's Guide

Notices

No part of this manual may be reproduced

in any form or by any means (including

electronic storage and retrieval or transla-

tion into a foreign language) without prior

agreement and written consent from Agi-

lent Technologies, Inc. as governed by

United States and international copyright

laws.

Manual Part Number

M8368-90011 Rev. D

Edition

11/2017

Printed in Germany

Agilent Technologies

Hewlett-Packard-Strasse 8

76337 Waldbronn

Warranty

The material contained in this docu-

ment is provided “as is,” and is sub-

ject to being changed, without notice,

in future editions. Further, to the max-

imum extent permitted by applicable

law, Agilent disclaims all warranties,

either express or implied, with regard

to this manual and any information

contained herein, including but not

limited to the implied warranties of

merchantability and fitness for a par-

ticular purpose. Agilent shall not be

liable for errors or for incidental or

consequential damages in connection

with the furnishing, use, or perfor-

mance of this document or of any

information contained herein. Should

Agilent and the user have a separate

written agreement with warranty

terms covering the material in this

document that conflict with these

terms, the warranty terms in the sep-

arate agreement shall control.

Technology Licenses

The hardware and/or software described in

this document are furnished under a

license and may be used or copied only in

accordance with the terms of such license.

Restricted Rights Legend

If software is for use in the performance of

a U.S. Government prime contract or sub-

contract, Software is delivered and licensed

as “Commercial computer software” as

defined in DFAR 252.227-7014 (June 1995),

or as a “commercial item” as defined in

FAR 2.101(a) or as “Restricted computer

software” as defined in FAR 52.227-19

(June 1987) or any equivalent agency regu-

lation or contract clause. Use, duplication

or disclosure of Software is subject to Agi-

lent Technologies’ standard commercial

license terms, and non-DOD Departments

and Agencies of the U.S. Government will

receive no greater than Restricted Rights as

defined in FAR 52.227-19(c)(1-2) (June

1987). U.S. Government users will receive

no greater than Limited Rights as defined in

FAR 52.227-14 (June 1987) or DFAR

252.227-7015 (b)(2) (November 1995), as

applicable in any technical data.

Safety Notices

CAUTION

A CAUTION notice denotes a

hazard. It calls attention to an

operating procedure, practice, or

the like that, if not correctly per-

formed or adhered to, could

result in damage to the product

or loss of important data. Do not

proceed beyond a CAUTION

notice until the indicated condi-

tions 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 indi-

cated conditions are fully

understood and met.

Software Revisions

This guide is valid for revision A.01.06 of

the Automated Purification Software in

combination with revision C.01.08 of the

OpenLAB CDS ChemStation Edition.

Purification Solution - Developer's Guide 3

In This Book

This manual contains instructions for Method Developers on how to use the

Automated Purification software.

1 The Role of the Method Developer

This chapter describes the role of the user of the Automated Purification

Software in Expert mode.

2 Preparing Default Purification Methods

This chapter describes the three default Purification methods that can be used

as a basis for the development of specific Purification methods.

3 Setting Up an Analytical and Preparative System

This chapter gives step-by-step instructions on setting up the analytical

system and the preparative system in the Automated Purification software.

4 Setting Up and Running a Purification Task

This chapter gives instructions for the most important steps for setting up and

running a Purification Task.

5 Reviewing Purification Results

This chapter describes how to review the results of a Purification Task.

6 Calibration Procedures

This chapter gives step-by-step instructions for the important calibration

procedures for the Purification system.

7 Checkout Procedure

This chapter gives step-by-step instructions on how to carry out a checkout

procedure to confirm the correct operation of your Purification system.

4 Purification Solution - Developer's Guide

Contents

1 The Role of the Method Developer 7

2 Preparing Default Purification Methods 9

General Method Settings 11

Analytical Method Settings 16

Preparative Method Settings 19

Agilent Active Splitter (G1968D/E/F) 23

Critical Method Parameters 24

3 Setting Up an Analytical and Preparative System 27

Setting up an analytical system 28

Setting up a preparative system 30

4 Setting Up and Running a Purification Task 33

Setting up a purification task 34

Configuring a new task 35

System Suitability Tests 38

Running a task 39

Processing partial data and cloning tasks 40

Reviewing analytical results 42

5 Reviewing Purification Results 43

6 Calibration Procedures 45

Characterizing the delay volumes: Mixing point to UV detector and Column to UV

detector 48

Characterizing the column volume 63

System Configuration and Delay Time Calibration 70

7 Checkout Procedure 83

Acquire an analytical run using the Chemstation sequence 85

UV-only Workflow: Focused gradient in the Purification software 89

Purification Solution - Developer's Guide 5

Contents

UV/MS Workflow: Focused gradient in Purification software 92

6 Purification Solution - Developer's Guide

Contents

Purification Solution - Developer's Guide

Agilent Technologies

The Role of the Method Developer

This chapter describes the role of the user of the Automated Purification

Software in Expert mode.

Purification software Method Developers work in Expert mode. They are

responsible for establishing the software work environment such that

Operators (working in Easy Prep mode) can use the purification software to

purify their samples.

This comprises the following tasks:

•Creating the (analytical and) preparative base methods that are used in the

instrument runs (see “Preparing Default Purification Methods” on page 9).

•Creating the analytical and preparative system parameter sets for all

analytical and preparative instruments and operating conditions that are

used by the Operators (see “Setting Up an Analytical and Preparative

System” on page 27). These systems should be named such that Operators

can easily identify their system. To retrieve system parameters, a set of

calibration procedures has to be executed, see “Calibration Procedures” on

page 45.

•Creating a set of purification task templates that are optimized for

purifying the sample types that are provided by the Operators (see “Setting

Up and Running a Purification Task” on page 33). We recommend that you

provide a task template for each combination of analytical and preparative

system that applies. Operators are expected to create their purification

tasks based on a Method Developer’s task template that matches their

system combination and separation needs.

•Creating a system suitability test task (see “System Suitability Tests” on

page 38) to verify that the instrument is still operating as expected. System

suitability tests can be executed by operators and method developers.

However, only method developers can accept a failed system suitability test

to release a blocked instrument.

•Instructing Operators on the work environment and how to set up and run

purification tasks.

8 Purification Solution - Developer's Guide

The Role of the Method Developer

In This Book

•Fixing problems (for example, adjusting parameters or target

identification) of Operators' tasks, to which the Operators do not have

access.

Method Developers have full access to all features of the purification software

and to the ChemStation while working within the main purification software

user interface (the purification task screen).

Purification Solution - Developer's Guide

Agilent Technologies

Preparing Default Purification Methods

General Method Settings 11

Analytical Method Settings 16

Preparative Method Settings 19

Agilent Active Splitter (G1968D/E/F) 23

Critical Method Parameters 24

This chapter describes the three default Purification methods that can be used

as a basis for the development of specific Purification methods.

This description summarizes the recommended purification method settings

for purification-related modules. Most of these method settings can be freely

modified according to your needs, with limitations noted in “Critical Method

Parameters” on page 24. For the alternative modules, which are not listed

here, use the applicable settings of the default modules.

Start with a new method:

• Method > New Method.

Methods settings are accessible from Instrument > Setup Instrument Method or

Method > Edit Entire Method.

NOTE

It is important for Purification software to mark the Save Method with Data check box in

Method > Runtime Check List.

NOTE

Switch off all pumps while you are setting up the methods.

10 Purification Solution - Developer's Guide

Preparing Default Purification Methods

In This Book

NOTE

It is highly recommended that the pumps are not switched off in a pre- or post-run

command of the method.

NOTE

Methods rely on the instrument configuration and driver revision. If you change the

instrument configuration or upgrade the driver revision for which you originally set up your

purification (base) method, you must at least save the method for the changed instrument

configuration under a new name. However, we recommend that, for a changed instrument

configuration or upgraded driver revision, you create a new method from scratch.

Otherwise, method resolution will try to adapt the methods from the old

configuration/driver revision with every method load (that is, for every sample run),

leading to a method changed state, and preventing the run going forward.

When creating a new task based on a task template with a different instrument

configuration, make sure that you choose an appropriate preparative base method for the

current instrument configuration and driver revision.

We recommend that you choose different task root folders for different instrument

configurations so that you do not mix different configurations in the same task root folder.

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