gpc/sec software for openlab cds

GPC/SEC Software for

OpenLab CDS

User Guide

GPC/SEC Software for OpenLab CDS User Guide

Notices

© Agilent Technologies, Inc. 2019

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Manual Part Number

D0000361

Edition

08/2019

Produced in Germany

Agilent Technologies, Inc.

Software Revision

This guide is valid for version 1.3 of the

Agilent GPC/SEC software for OpenLab

CDS

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Contents

GPC/SEC Software for OpenLab CDS User Guide 3

Contents

Contents 3

1. Introduction 5

2. Overview 9

3. Getting Started 15

4. Workflows 19

5. The GPC/SEC Processing Method 49

6. The GPC Results View 65

7. The GPC Distributions View 71

8. The GPC Calibrations Plot View 73

9. Reporting 75

10. Compliance 94

11. Exporting Information 98

12. Appendix 102

Contents

4 GPC/SEC Software for OpenLab CDS User Guide

This page is intentionally blank

Introduction


1. Introduction

Installation and configuration of the software is covered in the Installation Guide (G7860-90200) supplied with the software.

This manual will help you to familiarize yourself with the Agilent Technologies GPC/SEC software for the OpenLab CDS platform. It describes in detail the features and evaluation parameters of the software and contains the following information:

1 Overview

This chapter describes the general compatibility, configuration and features of the software.

2 Getting Started

This User Guide assumes a working knowledge of the OpenLab CDS platform for LC applications. This chapter outlines the areas of the OpenLab platform for which you need a basic level of understanding, and information about a GPC tutorial that provides you with an initial familiarization of the GPC/SEC software.

3 Workflows

This chapter describes the general workflows when using your software for GPC/SEC applications. They are broadly defined as:

▪ Using the Data Acquisition module to setup your instrument to collect data.

Introduction


▪ Using the Data Analysis module to perform processing of the collected data

This second section is broken down into the follow workflows:

▪ Defining a GPC/SEC Processing Method for GPC

▪ Generating a GPC Column Calibration using the three calibration options.

▪ Reviewing the GPC column calibration

▪ Processing a Sample Injection

▪ Reviewing Data & Results

4 The GPC/SEC Processing Method

This chapter describes the GPC specific additions to the processing method and goes into the detail of each of the GPC parameters, their function and dependencies.

5 The GPC Results View

This chapter describes the content and functions available in the GPC Results view which is added to the Results layout. This GPC specific view consists of the following tabs:

▪ The Peak Results Tab

▪ The GPC Column Calibration Tab

▪ The MW Ranges Tab

▪ The Percentage Fractions Tab

6 The GPC Distributions View

This chapter describes the content and functions available in the GPC Distributions view which is added to the Results layout.

7 The GPC Calibrations Plot View

This chapter describes the content and functions available in the GPC Calibrations Plot view which is added to the Results layout.

Introduction


8 Reporting

This chapter provides an overview of the options available, the GPC specific report items supplied by the software and the GPC and SEC specific report templates provided.

9 Compliance

This chapter provides an overview of the options provided by the GPC/SEC Software to allow the software to be used in a compliant environment.

10 Exporting Information

This chapter provides an overview of the options available to export GPC data and results in various standard formats.

11 Appendix

The Appendix provides information on:

▪ The function of the GPC License

▪ The default GPC & SEC Report Templates supplied.

▪ Additions to the OpenLab Platform

Introduction


Terms and Abbreviations

Table 1 Terms and Abbreviations used in this document

Term Description

CDS Chromatography Data System

AIC Agilent Instrument Controller – part of a distributed

Client/Server system

GPC Gel Permeation Chromatography

SEC Size Exclusion Chromatography

FRM Flow Rate Marker

Overview


2. Overview

The GPC/SEC software provides a data analysis module for conventional GPC/SEC calibration and calculations options which integrates into the Data Analysis component of the OpenLab CDS platform. The GPC/SEC software uses the existing workflows, processing options, data storage, reporting and compliance options supplied by the OpenLab CDS platform. It is able to process any signal from a concentration detector collected or imported into an OpenLab CDS project.

Compatibility

Target OpenLab Platform

Standard OpenLab CDS installation.

Configurations

All three OpenLab CDS configurations are supported:

▪ Workstation

▪ Workstation Plus

▪ Client/Server configuration

Overview


Instrument Control and Data Collection

The GPC/SEC software is purely a data analysis module, no additions or changes are made to the data acquisition part of the OpenLab platform.

The technique of GPC/SEC is an isocratic LC application (organic or aqueous) that uses GPC/SEC specific columns to perform the separation. This means any LC system supported by the OpenLab CDS platform that is capable of running in an isocratic configuration can be used.

Typical detectors used for GPC/SEC are:

▪ Refractive Index (RI)

▪ UV detector, Multiple wavelength (MWD), variable wavelength (VWD) and diode array (DAD)

▪ Evaporative Light Scattering Detector (ELSD)

▪ 3rd party via an analog to digital device

The detector required is dependent on the application.

The GPC/SEC software can process any chromatograms;

▪ Collected by the OpenLab Data Acquisition component of the platform

▪ Either into an OpenLab CDS project from the ChemStation, EZChrom or Galaxie platforms

Licensing

A GPC specific Data Analysis license is delivered as part of the GPC/SEC Data Analysis software.

▪ No GPC/SEC specific ‘Data Acquisition’ license is required

▪ The GPC/SEC license is provided in the standard 60-day startup license

▪ The GPC/SEC license is installed through the OpenLab Control Panel

One license provides a “seat” of GPC/SEC analysis on a Data Analysis workstation or client configured for GPC/SEC. If a GPC/SEC Analysis license is not available.

▪ The user is NOT able to perform “GPC/SEC processing”

Overview


▪ The GPC/SEC software will function as a ‘GPC/SEC Results reviewer’

GPC/SEC Features

The GPC/SEC software provides a data analysis module for conventional GPC/SEC calibration and calculations options. The core functions provided by the software are the ability to:

▪ Create and modify a GPC/SEC processing method

▪ Generate a new GPC/SEC column calibration

▪ Review an existing GPC/SEC column calibration

▪ Process injections using the GPC/SEC column calibration

▪ Review the results of existing processed injections

▪ Generate reports from one or more injection

"GPC /SEC Specific" Processing Method Type

A "GPC/SEC Specific" processing method type is added to the processing method options and is based on the standard GC/LC Area Percent method template provided by OpenLab. The GPC/SEC specific processing parameters are accessed from a “GPC specific” section of the method and are stored as part of the method.

GPC/SEC Column Calibration

A GPC/SEC processing method must be calibrated in order to perform GPC/SEC analyses on sample injections. A GPC column calibration is generated from injections identified with the Sample Type set as ‘Cal. Std.’. The GPC column calibration is stored as part of the processing method used. Only one GPC column calibration can exist for the method at any one time.

Overview


General GPC/SEC Options

The GPC/SEC software provides the ability to:

▪ Select the detector signal to be used for GPC processing. If multiple detector signals are collected for injections, the detector signal to be used can be selected. E.g. the Refractive index (RI) signal from an RI / UV combination or a single UV signal from multiple UV signals. To process sample injections, the detector signal used to generate a GPC Column Calibration must be present in the sample injections.

▪ Use Flow Rate Correction using the standard marker method.

▪ Use the Universal Calibration method to account for different polymer types between the calibrant(s) and samples to be evaluated.

GPC/SEC Column Calibration Options

A GPC column calibration can be generated using the following standard calibration methods:

▪ Narrow Standard Calibration

▪ Broad calibration options (Hamielec or Integral)

GPC/SEC Calculation Options

For each integrated peak, the following information can be calculated:

▪ The Molecular Weight (MW) Averages & Polydispersity (PD)

▪ The MW distribution plot

▪ The Cumulative distribution plot

▪ The percentage of material within defined MW limits

▪ The MW at specific peak fractions

Overview


GPC/SEC Results

The GPC/SEC software provides the ability to:

▪ View the table of MW averages and related information for one or a series of processed injections

▪ Overlay the chromatograms and derived plots (MW distribution & cumulative plot) for one or a series of injections

The processed injections can either be within the same results set or across results sets within the loaded project.

The GPC Results are stored as part of the processed injection.

Reporting

The OpenLab reporting tool can be used to create GPC specific report templates that provide the ability to generate:

▪ A report per sample injection

▪ A summary report for a series of injections

The processed injections can either be within the same results set or across results sets within the loaded project.

E.g.

▪ A table of MW averages for a series of injections

▪ Overlay of plots for a series of injections

GPC report items are supplied which comprise of a series of GPC specific tables and plots.

Two sets of default report templates are supplied, one set for typical GPC applications and the second for SEC applications.

Compliance

Storage of Parameters and Results

The GPC specific processing parameters, column calibrations, GPC results and report templates are all stored within the OpenLab CDS system.

▪ The GPC specific processing parameters and GPC column calibration are stored as part of the processing method

Overview


▪ The GPC Results are stored as part of the processed injection

Audit Trails

The GPC/SEC software hooks into the audit trails & diagnostics features within the OpenLab CDS system.

GPC Privileges & Roles

The GPC/SEC software uses the compliance, roles and privileges features of OpenLab Shared Services and provides three GPC specific privileges:

▪ Ability to edit GPC Parameters in a processing method

▪ Ability to create and modify a GPC column calibration

▪ Ability to perform a GPC analysis

The GPC specific privileges are assigned to default roles provided within the OpenLab CDS platform.

Export Options

The standard export features provided by OpenLab CDS are available within the various GPC specific windows and grids, allowing graphics (chromatograms, calibrations & distribution plots) and the contents of tables and grids to be exported to various standard formats.

In addition, an option is available which allows the GPC/SEC results of a processed injection to be exported as a simple ASCII file. The generated ASCII file can be loaded directly into Excel and provides access to the full GPC results and slice by slice data of the processed peak(s) within the injection.

Getting Started


3. Getting Started

Familiarity with the OpenLab CDS platform for LC Applications

This User Guide assumes a working knowledge of the OpenLab CDS platform for LC applications.

Before using the GPC/SEC software it is strongly recommended that you learn the basics of using your Agilent LC system with OpenLab CDS by following the interactive curriculum supplied in the OpenLab Help & Learning tool.

Home > Get Started > Getting Started > OpenLab CDS with LC This interactive curriculum covers the following topics.

User Interface Learn how to navigate the Control Panel and Acquisition interfaces to use your

system effectively. Topics include launching instruments, using and creating

custom layouts.

LC Acquisition

Methods

Learn how to manipulate acquisition methods to control your Agilent LC

instrument. Topics include modifying, saving, and downloading methods for

instrument control.

Run Submission Learn how to use your method to analyze samples to acquire data. Topics include

single sample analysis submission and using the run queue.

Data Analysis Learn how to create a processing method to generate results from your captured

data. Topics include result package overview, integration, compound identification,

and single level calibration.

Reporting Learn how to reprocess data and generate reports with your processing method.

Topics include using report templates to print single sample reports and make

basic template modifications.

Getting Started


Familiarization with the GPC/SEC Software

Once you are familiar with the basics of using your Agilent LC system, the GPC Help & Learning system should be used to familiarize yourself with the various functions & features of the GPC/SEC Software. The GPC Help & Learning system can be accessed from the program item OpenLab GPC Help or using F1 when focused on a GPC specific window or dialog. The Online Help has the following structure:

Getting Started

Familiarization with the GPC/SEC software

• Introduction to the GPC/SEC software

• Familiarization with the Data Analysis user interface

GPC/SEC Software Tutorial

This tutorial consists of a series of videos which guide you through the various aspects of the GPC/SEC software using a set of GPC/SEC data. This data is supplied on the GPC install media and can be imported into a project on your system. The tutorial covers the following:

• Aims of the tutorial

• Importing the GPC tutorial data into a project

• Viewing the tutorial data in the project

• Generating a GPC processing method

• Calibrating the GPC method using the narrow standards

• Processing the samples

• Reviewing the processed samples

• Reporting

Workflows

This section provides information about the general workflows.

▪ Data Acquisition

▪ Data Analysis

Getting Started


▪ Defining a GPC/SEC Processing Method

▪ Generating a GPC Column Calibration

• Creating a GPC Column Calibration (Narrow)

• Creating a GPC Column Calibration (Broad Hamielec)

• Creating a GPC Column Calibration (Broad Integral)

▪ Processing a Sample Injection

▪ Reviewing Data & Results

A series of topics that describe the GPC specific views and the parameters available. These can be accessed directly using the F1 key when focused on a GPC specific window or dialog.

▪ The GPC/SEC Processing Method

▪ The GPC Results View

▪ The GPC Distributions View

▪ The GPC Calibrations Plot View

▪ Reporting

Full information about the features and options available are described in the OpenLab Help & Learning tool. The following topics describe:

o GPC specific additions to the OpenLab Reporting module.

o The Default GPC & SEC Report Templates supplied.

Getting Started



Workflows


4. Workflows

The general workflow when using your software for GPC/SEC applications can be broadly defined as:

1 Using the Data Acquisition module to setup your instrument and collect data

2 Using the Data Analysis module to perform data analysis of the collected data

Data Acquisition

The GPC/SEC software is purely a data analysis module and does not provide any additional functionality to the Data Acquisition module. As the technique is an isocratic application (organic or aqueous) that uses GPC/SEC specific columns to perform the separation, any LC system supported by the OpenLab CDS platform capable of running in an isocratic configuration can be used.

The Use of Sample Types for GPC/SEC applications

The Sample Type ‘Cal. Std.’ is used by the software to identify injections that are GPC/SEC calibrants. This can be defined at time of data acquisition or can be set in the Injection List view in the Data Analysis program.

Workflows


Data Analysis

Once data is available to process in a project, the workflows for performing GPC/SEC analyses can be broadly summarized into the following:

1 Defining a processing method.

2 Generating a GPC column calibration from one or more calibrants linked to the processing method.

3 Reviewing the GPC column calibration.

4 Processing injections using the stored GPC column calibration linked to the processing method.

5 Reviewing the results of the processed injections.

Defining a GPC/SEC Processing Method

Defining a processing method can be broken down into the following key areas:

General Data Processing Parameters

The following parameters need to be defined:

Integrator to use A processing method can be setup to use either the ChemStation or

EZChrom integrators. The default option is the ChemStation integrator.

Integration Events Integration events need to be defined and fine-tuned for the acquired

data from your GPC instrument.

The manual integration option allows the integration of individual

peaks identified by the integrator to be changed by interactively

deleting the peak or editing the peak start, peak end, and peak

baseline.

System Suitability Optional, not required to perform GPC/SEC data analysis.

Tools Optional, not required to perform GPC/SEC data analysis.

Reports / Injection Report Optional. Define the report(s) required and destination for each

processed injection.

Workflows


GPC Specific Parameters

General Options

The following parameters on the GPC/GPC Method/General Tab need to be defined:

Signal to use Multiple detector signals can be collected for injections, but only one

detector signal can be processed by the GPC software at any one time.

E.g. the Refractive index (RI) signal from a RI / UV combination or a

single UV signal from multiple UV signals.

To process sample injections. the detector signal used to generate a

GPC Column calibration must be present in the sample injections.

Flow Rate Correction Optional.

This option allows injections to be corrected for variation in flow rate

using the standard marker method. To use flow rate correction, a

"marker component" must be included in all samples.

Universal Calibration Optional.

The Universal Calibration method can be applied to account for

different polymer types between the calibrant(s) used to generate a

GPC column calibration and the polymer samples to be evaluated. This

method requires Mark-Houwink constants, K and α (Alpha) values for

both sample and calibrants.

The default values provided are for Polystyrene in THF at ambient

temperature.

GPC Calibration Specific Options

Select the calibration method to generate the column calibration on the GPC/GPC Method/Column Calibration Tab:

Column Calibration Type Narrow Standard Broad Hamielec Broad Integral

Polynomial Curve Fit Select the order of fit Not applicable Select the order of fit

Cal.Std. Mark-Houwink parameters Optional Optional Optional

Peak Identification Tab Define this table Not applicable Not applicable

Broad Hamielec Parameters Tab Not applicable Define this table Not applicable

Broad Integral Tab Not applicable Not applicable Define this table

Workflows


The options above are described in more detail in the next section.

GPC Analysis Specific options

Two post data analysis options are available.

GPC/GPC Method/MW Range Tab If the percentage of material within specific MW ranges of an

integrated peak are required, then setup the parameters

required in this tab.

GPC/GPC Method/Percentage

Fractions Tab

If the molecular weights at specific percentage area fractions of

an integrated peak are required, then setup the parameters

required in this tab.

Save the processing method once all parameters have been defined.

NOTE Ensure all processing parameters are defined prior to processing injections either to

calibrate or evaluate samples. If any changes are made to the processing method after for

example, generating a GPC column calibration, then changes to the processing method

will make the GPC column calibration inconsistent with the processing method and any

processed injections will be marked as inconsistent. The injections of the GPC calibrants

will need to be reprocessed to regenerate the GPC column calibration

Workflows


Generating a GPC Column Calibration

The software provides three options of generating a GPC column calibration. These options are defined in the GPC/GPC Method/Column Calibration Tab of the processing method and are:

1 From a series of Narrow Standard Calibrants

Inputs:

RT of calibrant peaks

Mp of calibrant peaks

Polynomial curve order to apply

A series of “Narrow Standards” of

known peak MW (Mp)

GPC Column Calibration

Plot of Log(MW) –v- Peak RT

2 Using the Broad Hamielec Method

Inputs:

Target Mn & Mw averages

Target Tolerance

Maximum Number of Iterations

A “Broad Standard” of

known Mn & Mw



(curve fit order 1)

3 Using the Broad Integral Method

Inputs:

Integral table

(% Cumulative Weight Fraction

and Molecular Weight)

Polynomial curve order to apply

A characterized

“Broad Standard



The procedure to generate a column calibration depends on the selected calibration method. These procedures are described in the following section.

Workflows


The Use of ‘Sample Types’ for GPC

‘Sample Type’ In all three calibration methods, the ‘Sample Type’ should be set to Cal. Std. in the Injection List window for all injections that are to be used to generate a GPC column calibration.

‘Run Type’ When using a series of Narrow Standards to generate a GPC Column calibration, the ‘Run Type’ needs to be set to ‘Clear all calibration’ for the first of the calibrant of a series. This ensures that a new GPC column calibration is created.

Workflows


1 Creating a GPC Column Calibration (Narrow)

The most common method of generating a column calibration is to use a series of Narrow Standards. A series of narrow dispersity polymers from the same homologous series are dissolved in the eluent and injected on the column set. Each of the standards should have known Peak Molecular Weight (Mp) value. These values will have been provided on the certificate of analysis of the calibrants. The process of creating a GPC Column Calibration from a series of Narrow standards is a two-step process.

• Step 1 – Creating the Peak Identification Table

• Step 2 – Using the Peak Identification Table to generate a GPC Calibration

The process is summarized below.

Workflows


Step 1 – Creating the Peak Identification Table

The Mp values of the Narrow standards to be used for generating a GPC column calibration need to be predefined in the GPC processing method to be used by setting up a Peak Identification Table. This table needs to contain an entry for each calibrant consisting of, the expected retention time of the peak maximum and its associated Mp.

Narrow Standards Processing Method

Require a series of “Narrow Standards”

of known peak MW (Mp)

Identify the expected RT values of calibrants & assign

the Mps from the certificate of analysis of the

calibrants.

Define the curve fit to apply

Peak Identification Table

Stored in the processing method

This Peak Identification Table provides the ability to pre-define a calibration template of calibrants in a GPC processing method. This processing method can be stored as a master method for a specific GPC application. This master method provides the ability to generate a column calibration without the need for an operator to manually define the Mp values of the calibrant set.

Workflows


Step 2 – Using the Peak Identification Table to generate a GPC Calibration

Once the Peak Identification table has been completed, this ‘template’ can be used to generate a GPC column calibration either from the set of calibration standards used to define the Peak Identification table, or from subsequent injections of the same calibrant set run under the same chromatographic conditions.

Processing Method

Peak identification table

Narrow Standards

Process the Calibrants




The process to generate a GPC column calibration using narrow standards is described below.

Step 1a Setup the GPC processing method

Step 1b Define the Peak Identification Table in the processing method

Step 2a Create the column calibration

Step 2b View the generated column calibration

Step 2c Fine tune the column calibration

Workflows


Step 1a. Setup the GPC Processing Method for Narrow Standard Calibration

Setup the processing options as described above. The key GPC parameters are:

GPC/GPC Method/General Tab

1 Select the default detector signal to use.

2 Decide if you want to use flow rate correction.

3 If using the Universal Calibration option, define the Mark-Houwink values for the samples.

GPC/GPC Method/Column Calibration Tab

1 Select Calibration type Narrow Standard.

2 Select the curve fit to apply to the calibration data points.

3 If using the Universal Calibration option, define the Mark-Houwink values for the calibrants.

Save the processing method.

Ensure the calibrant injections to be used are linked to the GPC processing method to be calibrated.

Workflows


Step 1b. Defining the Peak Identification Table in the Processing Method

There are two methods of defining this table.

Interactively from a set of calibrants

The method requires a set of injections of the narrow standards that are to be used under these conditions. The injections need to be either integrated using the automated integrator to identify the calibrant peaks or, defined using the manual integration tool.

For the Calibrant set:

1 Select the Chromatogram view and define the start and end of each peak and the software will determines the peak maxima of each calibrant. The peak start and end do not need to be defined exactly as it is only the retention time at the peak maximum that is required for each peak.

2 If using flow correction, ensure the expected peak maximum of the flow marker component has been defined in the GPC/General tab of the processing method.

For each calibrant:

1 Select the Peak Identification Tab in the Method View/GPC/GPC Method section.

2 Ensure the first calibrant is selected in the run list and right click in the Peak Identification Tab area.

3 Select Add peaks from chromatogram from the right click menu. The peaks identified in the injection will be added to the Peak Identification table of the processing method.

4 Assign the Mp for each peak to be used. It doesn't matter if peaks identified in the chromatogram are added to the Peak Identification table that are not from the Narrow Standards. These peaks can be either deleted from the final Peak Identification table or ignored. Any peaks in the table which have not been assigned MW value are ignored by the system when generating a GPC column calibration.

Workflows


5 Define the Peak Identification Window. The criteria for peak identification is; The expected retention time of the peak +/- [(The Retention Time window) / 2]. The default value is 0.1 minute giving a default window of +/- 3 seconds.

6 Repeat the process for each subsequent narrow standard calibrant

Manual entry of the parameters from a set of calibrants

The method requires a predetermined table of the expected peak retention times and their associated Mp values.

For the calibrant set:

1 In the Method View, select the /GPC/GPC Method/Peak Identification Tab.

2 Enter the retention time of the peak maximum of each calibrant peak and its associated Mp value.

3 Define the Peak Identification Window. The criteria for peak identification is; The expected retention time of the peak = +/- [(Retention Time window) / 2]. The default value is 0.1 minute giving a default window of +/- 3 seconds.

Once the peak identification table has been completed, save the processing method.

If not already done so, ensure the injections are linked to the processing method.

Workflows


Step 2a. Creating the GPC Column Calibration

Select the Injection List and ensure the ‘Sample Type’ is set to ‘Cal. Std.’ for the injections to be used to generate the GPC column calibration.

For the first of the calibrant injections to be used, ensure the ‘Run Type’ is set to ‘Clear all calibration’

In the Run List, select all the calibrants.

Select ‘Reprocess selected injections’.

Any peaks identified in each of the calibrants injections which match the peak retention time values in the Peak Identification Table are assigned with the associated Mp from the Peak Identification Table and added to the GPC column calibration.

Processing Completed

On completion of processing all ‘Cal. Std.’, the data points are added to the GPC Calibration Points table and the curve fit defined in the method applied to the data points.

The column calibration has now been created and can be reviewed.

Workflows


Step 2b. Viewing the Generated GPC Column Calibration

The tabs in the GPC Column Calibration node of the GPC method can now be used to view the calibration.

The GPC Calibration Points Tab Displays the current column calibration data points table and

associated parameters.

The GPC Calibration Plot Tab Comprises of a read only plot of the data displayed in the GPC

Calibration Points Tab.

The GPC Calibration Details Tab Displays details about the column calibration data and how it

was derived.

Step 3c. Fine Tuning an Existing GPC Narrow Standard Column Calibration

If the generated calibration requires modification, for example,

▪ Change to the curve fit

▪ Deselection of calibration data points

▪ Addition or deletion of a data point

▪ Change to the MW of a data point

▪ Change to the Mark-Houwink K and Alpha parameters

▪ Change to the flow rate marker retention time

Any changes need to be made to the processing method and the calibrants reprocessed to regenerate the calibration using the new set of parameters.

Workflows


2 Creating a GPC Column Calibration (Broad Hamielec)

This method requires the use of a Broad Standard of known Mn and Mw averages and generates a linear calibration. The software performs a trial and error search such that the calculated values of Mn and Mw match those documented for the Standard.

The process of creating a GPC Column Calibration using the Broad Hamielec method is a two-step process.

Step 1 – Define the Processing Method

The target MW averages (Mn and Mw), the Maximum Number of Searches and the Tolerance Value for Mn and Mw, expressed as a percentage of those Molecular Weights need to be defined in the Broad Hamielec Parameters tab of the processing method to be used.

Broad Standard Processing Method

Require a “Broad Standard”

of known peak Mw & Mn

Define:

The target MW Averages (Mn & Mw)

from the certificate of analysis of the calibrant

The Target Tolerance

The Maximum Number of search Iterations

Broad Hamielec Parameters


Workflows


Step 2 – Process the Calibrant to generate a GPC Calibration

The Broad Hamielec Parameters are then used to create a column calibration from the calibrant.

Processing Method

Broad Hamielec Parameters

Broad Standard




Polynomial curve order 1 applied. (fixed)


The process to generate a GPC column calibration using the Broad Hamielec method is described below.

Step 1a Setup the processing method

Step 1b Define the Broad Hamielec Parameters in the processing method

Step 2a Create the GPC column calibration

Step 2b View the generated GPC column calibration

Step 2c Fine tune the column calibration

Workflows


Step 1a. Setup the GPC Processing Method for Broad Hamielec Calibration







1 Select Calibration Type Broad Hamielec.

2 If using the Universal Calibration option, define the Mark-Houwink values for the calibrant.

Step 1b. Defining the Broad Hamielec Parameters in the processing method

Select the Broad Hamielec Parameters Tab and define the following:

1 The target Mn Average & Mw Average from the certificate of analysis of the calibrant.

2 The target tolerance.

3 The maximum number of search iterations.


Ensure the calibrant injection to be used is linked to the processing method to be calibrated.


Select the Injection List and ensure the ‘Sample Type’ is set to ‘Cal. Std.’ and the ‘Run Type’ to ‘Clear all calibration’ for the injection to be used to generate the GPC column calibration.

Note:

If the Injection List was setup prior to creating the method then would not need to reprocess the calibrant. The calibrant would have been analysed and the calibration created on linking the method.

Workflows


In the Run List, select the calibrant.




The tabs in the GPC Column Calibration node of the GPC method can now be used to view the calibration. A calibration generated using the Hamielec method will consist of a straight-line fit with two data points indicating the retention time limits of the calibrant used.






was derived.

Step 2c. Fine Tuning an Existing Broad Hamielec Column Calibration

If the generated calibration requires modification, edit the parameters in the Broad Hamielec Parameters Tab and reprocess the calibrant.

Workflows


Creating a GPC Column Calibration (Broad Integral)

This method requires the use of a single well characterized Broad Standard, i.e. with a large dispersity value to calibrate the column set. The standard to be used must have a table detailing the % Cumulative Weight Fraction and either Log Molecular Weight or Molecular Weight values supplied by the manufacturer of the standard.

The process of creating a GPC Column Calibration using the Broad Integral method is a two-step process.

Step 1 – Define the Processing Method

Broad Standard Processing Method

Requires a characterized

“Broad Standard”

Enter the Integral table

(% Cumulative Weight Fraction and Slice Molecular

Weight) supplied on the certificate of analysis of

the calibrant

Define the curve fit to apply

Broad Integral Setup


Workflows


Step 2 – Process the Calibrant to generate a GPC Calibration

The Broad Integral table is then used to create a column calibration from the calibrant.

Processing Method

Broad Integral Setup

Broad Standard





The process to generate a GPC column calibration using the Broad Integral method is described below.

Step 1a Setup the processing method

Step 1b Define the Broad Integral table in the processing method

Step 2a Create the GPC column calibration

Step 2b View the generated GPC column calibration

Step 2c Fine tune the GPC column calibration

Workflows


Step 1a. Setting up the Processing Method for Broad Integral Calibration







1 Select Calibration Type Broad Integral. The “Polynomial curve fit” parameter is displayed and the "Broad Integral Setup Tab" is displayed.

2 Select the default curve fit to apply to the calibration data points.

3 If using the Universal Calibration option, define the Mark-Houwink values for the calibrant.

Step 1b. Broad Integral Setup Tab

This tab consists of a grid containing Slice Mp (g/mol), Percentage Weight data pairs.

Enter the Integral table (% Cumulative Weight Fraction and Slice Molecular Weight) supplied on the certificate of analysis for the calibrant. If the integral table is available as a text file with the format:

<Slice MW value 01 <tab> <Percentage Weight value 01>


…

<Slice MW value N <tab> <Percentage Weight value N>

Workflows


This text file can be copied to the Windows clipboard and using the Paste option available in the Right Click menu of the Broad Integral Setup grid, pasted into the table below the current last row of the table. Any rows without the tab separator are ignored. Alternatively, the data table can be entered manually by using the Add broad integral option available on the right click menu. Options are available in the right click menu of the Broad Integral Setup grid which allow rows to be added and deleted.


Ensure the calibrant injection to be used is linked to the processing method to be calibrated.


Select the Injection List and ensure the ‘Sample Type’ is set to ‘Cal. Std.’ and the ‘Run Type’ to ‘Clear all calibration’ for the injection to be used to generate the GPC column calibration.

In the Run List, select the calibrant.


NOTE:

If the Injection List was setup prior to creating the method then would not need to reprocess the calibrant. The calibrant would have been analysed and the calibration created on linking the method.


Workflows



The tabs in the GPC Column Calibration node of the GPC method can now be used to view the calibration.






was derived.

Step 2c. Fine tuning an Existing Broad Integral Column Calibration

If the generated calibration requires modification, for example,

▪ Change to the curve fit

▪ Deselection of calibration data points

▪ Addition or deletion of a data point

▪ Change to the MW of a data point

▪ Change to the Mark-Houwink K & Alpha parameters

▪ Change to the flow rate marker retention time

Any changes need to be made to the processing method and the calibrants reprocessed to regenerate the calibration using the new set of parameters.

Workflows


Processing a Sample Injection

Once a GPC processing method has been calibrated, injections can be processed using this method. The procedure to process a sample injection is the same regardless of the method of calibrating the system.

Sample GPC/SEC Results

The ‘Molecular Weight Averages’

Number Average (Mn), Weight Average (Mw), Mz,

Mz+1

+ Polydispersity (Mn/Mw)

+

The ‘Molecular Weight Distribution Plot’

The ‘Cumulative Plot’

Optional

The % of the sample peak within defined MW

limits

The MW at specific % peak fractions

Each injection can be processed in turn or, all injections in a sequence can be processed automatically.

The procedure to process an injection is described below.

Workflows


Setting up the GPC Processing Method

NOTE The GPC processing method needs to be fully defined before calibrating the processing

method, as any change to the processing method after generating of a GPC column

calibration will make the calibration inconsistent with the processing method, the

calibration will need to be recreated and any processed injections will be marked as

inconsistent.

The key GPC parameters are:


1 Select the detector signal to use.


3 If using the Universal Calibration option, ensure the Mark-Houwink values for the samples have been defined.

Parameters

Optional GPC/GPC Method/MW Ranges & Percentage Tabs

If this information is required, ensure the parameters have been defined and the options switched on.

‘Sample Type’

Select the Injection List and ensure the ‘Sample Type’ is set to ‘Sample’ for the injections to be processed.

Process the Injection

In the Run List, select the injection to be processed.


The GPC/SEC results are calculated for each integrated peak in the defined signal of the selected injection.

Workflows


Viewing the GPC Results

The results for the processed injection are available in the GPC specific views which are accessed from the Results Layout View. The GPC specific views comprise of:


▪ The GPC Distributions Plot View

▪ The GPC Calibration Plot View

The GPC Results View

This view comprises of the following tabs:

The Peak Results Tab Consists of a grid containing the calculated MW Averages for

each integrated peak in the selected processed Injection.

The GPC Column Calibration Tab Displays the column calibration used to process the selected

injection. The content is the same as the GPC Column Calibration

Details tab accessed from the processing method.

The MW Ranges Tab Displays the MW Ranges calculated from each integrated peak in

the selected processed injection. It is only populated if the GPC

MW Ranges option is switched on in the processing method.

The Percentage Fractions Tab Displays the MW at the specific % fractions defined in the

method from each integrated peak in the selected processed

injection. It is only populated if the GPC Percentage Fractions

option is switched on in the processing method.

The GPC Distributions Plot View

The GPC Distribution Window displays the MW distribution plot(s) and optional cumulative plot(s) for the selected injection. If the processed injection contains more than one processed peak, all the distribution plots are displayed on the same axes.

Workflows


The GPC Calibrations Plot View

The GPC Calibrations Window displays the GPC column calibration used to process the injection.

Peak Integration limits

The peak integration limits for an injection can be modified using the Manual integrator tool option available in the Chromatograms window.

Modifying the integration limits of a peak will automatically reprocess the sample.

At the end of the analysis process Save All Results by clicking on the Save All Results Icon, located in the Processing Toolbar via the Home or Processing Tabs.

This is good practice before closing the result set and project.

Workflows


Reviewing Data & Results

The results of processed samples in a result set can be viewed at any time.

Results from an injection

Select the Results Layout Tab and select the processed injection in the run list.

The results of a processed sample can be accessed from the various GPC windows and tabs.


▪ The GPC Distributions View

▪ The GPC Calibration Plot View

Selecting another sample injection in the run list will update the display with the results from that sample.

Results from a series of injections

The results of a series of process injections can be reviewed and overlaid. The key to reviewing results is the use of the Pin function and the concept of the focused injection (The current selected injection, if a series of injections are selected)

Select the injections to be compared using the Pin function. (The processed injections can be from the same or different results sets.). The selected injections and results are now displayed in the various results windows.

The Chromatograms view

The selected signals of the pinned injections are displayed in the Chromatograms View.

Workflows



The GPC Results Window displays the calculated MW Averages and related results for all the selected injections.

The Peak Results Tab Displays the calculated MW Averages and related parameters

for each peak in each pinned injection.

The GPC Column Calibration Tab Displays the GPC calibration parameters used to process the

focused injection.

The MW Ranges Tab Displays the MW Ranges calculated from each integrated peak

in the pinned injections. It is only populated if the GPC MW

Ranges option is switched on in the processing method.

The Percentage Fractions Tab Displays the MW at the specific % fractions defined in the

method from each integrated peak in the pinned injections. It is

only populated if the GPC Percentage Fractions option is

switched on in the processing method.

The GPC Distributions Window

The Distribution Plot Tab displays the MW distribution plot(s) and optional cumulative plot(s) for each integrated peak in the selected injection. The distribution plots of all injections are displayed on the same Log MW axis.


The GPC Calibrations Window displays the GPC column calibrations used to process the pinned injections.

Workflows


The GPC Column Calibration used to process a sample

The GPC column calibration used to process a sample injection is stored within the sample injection results.

Display the Results Layout View and select the processed injection in the run list.

The column calibration details used to process the selected injection can be accessed from the GPC Column Calibration Tab in the GPC Results View.

A plot of the GPC column calibration can be accessed from the GPC Calibrations Plot View.

Current Column Calibration of a Processing Method

The Current GPC column calibration of a processing method can be viewed from the GPC/GPC Column Calibration section of the processing method.

The GPC Calibration Points Tab Displays the current column calibration data points table

and associated parameters.

The GPC Calibration Plot Tab Comprises of a read only plot of the data displayed in

the GPC Calibration Points Tab.


was derived.

The GPC/SEC Processing Method


5. The GPC/SEC Processing Method

This section describes:

▪ The GPC specific additions to the processing method

▪ The GPC parameters and their function

The GPC/SEC software provides a "GPC Specific" processing method type based on the method type ‘GC/LC Area Percent’ and supports:

▪ Integration and Area% / Height% calculation

▪ Signal alignment

▪ Blank subtraction for GC, LC, A/D data

▪ System suitability

▪ GPC column calibration

▪ Calculation of molecular weight averages & distribution plot

▪ Calculation of % Material within specific MW ranges

▪ Calculation of Mw information at specific % Fractions

▪ Custom calculation

▪ Reporting



The GPC parameters are accessed from the GPC section of the processing method which is added to the bottom of the processing method section. The parameters are displayed in two sub sections:

1 GPC/GPC Method

2 GPC/GPC Column Calibration

All GPC parameters are stored as part of the Data Analysis processing method.

The GPC Method Section

This section provides access to GPC specific parameters for:

1 Generating a GPC column calibration

2 Processing an injection using a GPC column calibration

The GPC parameters are accessed via a series of tabs. The tabs that are displayed depend on the ‘Column Calibration type’ selected in the ‘Column Calibration’ tab.

Tab Comments

General

These tabs are common for all GPC column calibration types. Column Calibration

MW Ranges

Percentage Fractions

Peak Identification This tab is only displayed when Narrow Standard column

calibration type is selected.

Broad Hamielec Parameters This tab is only displayed when Broad Hamielec column calibration

type is selected.

Broad Integral Setup This tab is only displayed when Broad Integral column calibration

type is selected.



The General Tab Parameters

The parameters on the General tab are:

▪ Signal

▪ Flow Rate Correction

▪ Use flow rate correction check box

▪ FRM name

▪ Expected RT

▪ RT window

▪ Sample Mark-Houwink Parameters

▪ K((10e-5) dL/g)

▪ alpha

General/Signal

This parameter is used to identify the chromatogram detector signal to be used when processing an injection. The drop-down menu displays a list of the detector signals available in the currently selected injection/results set. When the Process / Reprocess Injections option is used, the selected signal in the injection is processed. How the injection is processed is dependent on the Sample Type defined in the Injection List as follows.

Sample type Action

‘Cal. Std’ When the defined ‘detector signal’ exists in the injection, the injection is used to

create / update a GPC column calibration.

‘Sample’ &

others types

When the defined ‘detector signal’ exists in the injection, the injection is processed

using the GPC calibration associated with the processing method (when it exists).

In both cases, when the defined ‘detector signal’ does not exist in the injection, the

injection is ignored.

Flow Rate Correction/Flow Rate Marker Name

This option provides the ability to enter the name of the component used in the sample injections for the flow marker indicator.



Flow Rate Correction/Expected RT

This parameter defines the expected peak retention time of the “flow rate marker peak”. It is used in conjunction with the RT window to identify the flow rate marker component in an injection. When using the flow rate correction option, the following two parameters need to be defined.

Flow Rate Correction/RT window

This parameter defines the Retention Time search window to identify the flow rate marker peak in an injection. The system will attempt to identify a peak in an injection sample which is +/- [(Retention Time window) / 2] minutes of the Expected Retention Time value for the flow marker stored in the processing method being used. The default value is 1.000 minutes (+/- 30 second window.)

Sample Mark-Houwink Parameters

The Universal Calibration method can be used to account for different polymer types between the calibrant(s) used to generate a GPC column calibration and the polymer samples to be evaluated. These constants vary with polymers type, solvent and temperature. Tables listing these constants for a wide variety of polymers in different solvents are available in literature.

Parameter Description

K The value of K that will be used in the GPC calculations when processing a sample.

Minimum value 0.01 Maximum value 9999.999

Default value 14.100 Units (10e-5) dL/g

Alpha The value of Alpha that will be used in the GPC calculations when processing a sample.


Default value 0.700 Units none

The default values provided are for Polystyrene in THF at ambient temperature. The Mark-Houwink constants for the calibrants are defined in the Column Calibration tab.



The Column Calibration Tab Parameters

The parameters on the Column Calibration Tab are:

1 Column Calibration Type

2 Cal. Std. Mark-Houwink Parameters

Column

Calibration Type Description

Narrow Standard Require a series of Narrow Standards of known Mp.

When this option is selected:

The “Polynomial curve fit” parameter is enabled

The "Peak Identification Tab" is displayed

Broad Hamielec This method utilizes a Broad Standard with known Mn and Mw and assumes

that the calibration to be generated is linear. The software performs a trial and

error search such that the calculated values of Mn and Mw match those

documented for the Standard. The Maximum Number of Searches, and Tolerance

Value for Mn and Mw, expressed as a percentage of those Molecular Weights

need to be defined in the processing method to be used.


The "Broad Hamielec Parameters Tab" is displayed

Broad Integral This method requires a characterized Standard with known MW at specific Wt%.

A Broad Standard calibration involves the use of a single well characterized

Broad Standard, i.e. with a large dispersity value to calibrate the column set. The

standard to be used must have a table detailing the % Cumulative Weight

Fraction and either Log Molecular Weight or Molecular Weight values supplied

by the manufacturer of the standard.


The “Polynomial curve fit” parameter is displayed with values 1 to 5

enabled.

The "Broad Integral Setup Tab” is displayed

Polynomial curve fit

This parameter defines the type of curve fit (1st order to 5th order) that will be applied to a new column calibration using the Narrow Standard or Broad Integral method. For a Hamielec calibration, a 1st order polynomial is automatically applied and cannot be changed.



Cal. Std. Mark-Houwink Parameters

The Universal Calibration method can be applied to account for different polymer types between the calibrant(s) used to generate a GPC column calibration and the polymer samples to be evaluated. This method requires Mark-Houwink constants, K and α (Alpha) values to be the same for both calibrants and sample polymer types. These constants vary with polymers type, solvent and temperature. Tables listing these constants for a wide variety of polymers in different solvents are available in literature.


K The value of K that will be used when generating a GPC column calibration.


Default value 14.100 Units (10e-5) dL/g

Alpha The value of Alpha that will be used when generating a GPC column calibration.


Default value 0.700 Units none

The default values provided are for Polystyrene in THF at ambient temperature. The Mark-Houwink constants for the samples are defined on the General tab.



The Peak Identification Tab

This tab is only displayed when the Column calibration type in the Column Calibration tab is set to “Narrow Standard”.

This tab is used to define a set of Peak Retention times versus MW values for the peaks of the narrow standard calibrants to be used to generate a GPC column calibration. This tab consists of a grid containing the following parameters.


RT (min) The expected peak retention time of a calibrant peak

MW (g/mol) The MW to be assigned to the calibrant peak

Peak RT window (min) The retention time search window to identify the calibrant peak (+/-

[(Retention Time window) / 2. The default value is 0.1 mins (+/- 3 seconds)

Sample name The name of the injection from which the data point has been added.

Signal The detector signal name of the injection from which the data point has been

added

Source chromatogram The source chromatogram of the injection from which the data point has

been added.

Source chromatogram

data sequence

The data sequence containing the source chromatogram.

Source chromatogram

project

The name of the project containing the source chromatogram data sequence.

Use point Defines if the point is to be included in the calculation of the line of fit of the

GPC calibration

The options available are:

▪ Automatic entry of peak retention time from actual calibrant injections and subsequent manual entry of the associated MW values.

▪ Manual entry of the expected retention time, retention time window and associated MW value of the calibrants.



Right Click menu options

Options “Choose columns…”, “Numeric precision…”, “Copy to clipboard” and “Export

to file…”

The following GPC specific items are available on the right click menu of the Peak Identification Table:



Command Description

Add peaks from

chromatogram

Adds the peaks currently identified in the selected injection to the Peak

Identification table populating the parameters in the table.

The MW for each peak is assigned as 0 by default.

Add peak A calibration point can be defined manually by adding a row to the Peak

Identification table. The Peak Retention Time and MW parameters are set to

0.

The following parameters can be defined for a row:

Peak Retention Time

MW

Peak Retention Time window

Use point

Delete selected

peak(s)

Deletes the currently selected row or rows in the table.

The Broad Hamielec Parameters Tab

This tab is only displayed when the Column calibration type in the Column Calibration tab is set to “Broad Hamielec".

This method utilizes a Broad Standard with known Mn and Mw. The Hamielec method assumes that the calibration to be generated is linear. The software performs a trial and error search such that the calculated values of Mn and Mw match the target values documented for the Standard. The Maximum Number of Iterations together with a Target Tolerance Value for Mn and Mw, expressed as a percentage of those Molecular Weights need to be defined in the Processing method to be used. This tab is used to define the Hamielec MW and Search Parameters and consists of:


Target Mn Average Target Mn Average of the calibrant injection to be used

Target Mw Average Target Mw Average of the calibrant injection to be used

Target tolerance The target tolerance expressed as a percentage of the known Molecular

Weights


Default value 5.00 Units %



Maximum Number

of Iterations

The maximum number of iterations to use in the search process to determine

the best calibration line to achieve the target Mn & Mw values within the

defined target tolerance.

Minimum value 1 Maximum value 99999

Default value 5 Units n/a

If the target molecular weight or tolerance are not achieved, the calibration is still generated but a warning message will be displayed to indicate the calculation process has been terminated. The calibration that is created is identified with two data points to indicate the retention time limits of the calibrant used, it can be reviewed in the Column Calibration View.

The Broad Integral Setup Tab

This tab is only displayed when the Column calibration type in the Column Calibration tab is set to “Broad Integral”.

This method requires a broad standard that has been characterised with a minimum number of 5 fractions to generate a cumulative molecular weight table. This tab is used to define the Integral table detailing the % Cumulative Weight Fraction and either Log Molecular Weight or Molecular Weight values supplied by the manufacturer of the standard. This tab consists of a grid containing Slice MW (g/mol), Percentage Weight data pairs.


Percentage Weight Defines the percentage weight fraction of the MW slice



Slice MW (g/mol) The MW for the corresponding percentage weight fraction.

Minimum value 0 Maximum value 99,999,999

Default value 0 Units g/mol


Options “Choose columns…”, “Numeric precision…”, “Copy to clipboard” and “Export

to file…”



The following GPC specific items are available on the right click menu:

Command Description

Paste Pastes the contents of the clipboard into the table below the current last row of

the table. The contents of the clipboard must have the format:



…

<Slice MW value N <tab> <Percentage Weight value N>

Any rows without the tab separator are ignored.

Add broad integral Adds a row to the bottom of the existing table with the default values for the

Slice MW & Percentage weight fraction.

Delete selected

broad integral(s)

Deletes the currently selected row(s) from the table.

(No confirmation dialog is displayed).

The MW Ranges Tab

This option allows the calculation of the % of material within specific MW ranges when performing a MW distribution calculation. Any number of MW Ranges can be defined in this dialog. The results are provided in the MW Ranges tab of the GPC Results View accessed from within the Results Tab.


MW Ranges

Checkbox

Provides the ability to enable/disable the calculation of the defined MW

Ranges when processing Injections. The Ranges can be defined/edited even if

the checkbox is unchecked.

High MW limit

(g/mol)

This is the high molecular weight limit of the MW range to be calculated.

The value "M+" can be used to define the Maximum Molecular Weight of an

injection.

Low MW limit

(g/mol)

This is the low molecular weight limit of the MW range to be calculated.

The value "M-" can be used to define the Minimum Molecular Weight of an

injection.

MW Range Name An optional text label that provides a way to identify specific MW ranges in a

report.



If the entered low limit is greater than the entered high limit, then the following error message is displayed. “Error. The low limit MW value must be less than the high limit MW value” The previous value is restored after clicking OK.

If the entered high limit is greater than the entered low limit, then the following error dialog is displayed. “Error. The high limit MW value must be greater than the low limit MW value”. The previous value is restored after clicking OK

Right Click Menu Options


Command Description

Copy to Clipboard Copies the whole table with headers to the clipboard as tab separated text.

Example of contents:

High MW limit (g/mol)

M+

100000

Low MW limit (g/mol)

100000

1000

Add MW Range Adds a row to the bottom of the current table with the values set to the

default values M+ to M-.

Delete selected MW

range(s)


The Percentages Fractions Tab

This option allows the calculation of the molecular weights at specific percentage area fractions of an injection peak. E.g. Calculate the molecular weights at the first 10% of the peak area and at the last 10% of the peak area. Any number of fractions can be defined. The High Fraction & Low Fraction % values do not need to be the same values. The results are provided in the Percentage Fractions Tab of the GPC Results View accessed from within the Results Tab.


Calculate

percentage fractions

Provides the ability to enable/disable the calculation of the percentage

fractions when processing Injections. The fraction ranges can be defined/edited

even if the checkbox is unchecked.



High fraction % The percentage fraction from the peak start retention time at which to calculate

the molecular weights for:



Low fraction % The percentage fraction from the peak end retention time at which to calculate

the molecular weights for.



Right Click Menu Options

The following GPC specific items are available on the Right Click menu:

Command Description

Copy to Clipboard Copies the whole table with headers to the clipboard as tab separated text.

Example of contents.

High fraction % Low fraction %

10.0 10.0

5.0 20.0

Add fraction Adds a row to the bottom of the current table with the values set to the

default values 0.0 to 0.0.

Delete selected

fraction(s)




The GPC Column Calibration Section

This section provides access to the GPC calibration associated with the processing method. The GPC column calibration parameters are accessed via three tabs:

1 GPC Calibration Points tab

2 GPC Calibration Plot tab

3 GPC Calibration Details tab

The GPC Calibration Points Tab

The contents of this tab comprise of a read only grid which displays the current Calibration Data Points Table and associated parameters. The content of this grid is the same for all three GPC calibration types.


Assigned MW (g/mol) Narrow

Standard

The MW value corresponding to the RT value of the peak

nearest to the entry in the Peak Identification table.

Hamielec The MW value corresponding to the start and end points

of the calculated line of fit.

Integral The Slice Mp for the individual fractions.

FRM RT (min) The retention time of the flow marker identified in the Injection. When the

flow rate correction option is not selected then 0.000 is displayed.

log MW The log value of the assigned MW value.

Percent error The percentage error of the data point derived from the line of best fit being

applied.

Predicted MW (g/mol) The calculated MW from the line of best fit at the Retention Time of the data

point.

Residual The residual error of the data point derived from the line of best fit being

applied.

RT actual (min) The actual Retention Time of the peak in the calibrants injection.

RT corrected (min) The flow rate corrected Retention Time of the peak in the calibrants injection.

When the flow rate correction option is not selected then this value is the

same as the RT actual.

Sample name The sample name of the injection from which the calibrant data point was

obtained.



Signal The signal used in the injection from which the calibrant data point was

obtained.

Source chromatogram The source chromatogram of the injection from which the data point has

been added.

Source chromatogram

data sequence

The data sequence containing the source chromatogram.

Source chromatogram

project

The name of the project containing the source chromatogram data sequence.

The GPC Calibration Plot Tab

This tab comprises of a read only plot of the data displayed in the GPC Calibration Points tab.

Plot Contents Log MW -v- RT corrected (min)

The data points are displayed as blue circles

The calculated line of fit is displayed in red

Y Axis scale Log X Axis scale Linear

Y Axis title MW (g/mol) X Axis title Retention time (min)

Y Axis units g/mol X Axis units Minutes

Legend Displays the name of the processing method

Functions available

The following GPC/SEC specific items are available:

Command Description

Expand/Collapse Each of the sections can be collapsed or expanded.

Tooltip When the mouse cursor is over a data point in the calibration plot, a tool tip

displays the following information:

• The retention time (min) of the data point.

• The MW (g/mol) assigned to the data point.

• The sample name of the source chromatogram.

• The filename of the source chromatogram.

The values are taken from the current GPC column calibration displayed in the

GPC Calibration Points tab of the method.



Right Click menu

Auto Scale Autoscales the plot.

Copy to clipboard Clipboard as a tab separated text.

Export to file Saves the displayed information AND the calibration data points table to the

file.

The GPC Calibration Details Tab

This tab displays details about the column calibration data and how it was derived. The content depends on the GPC calibration type.

Functions available

The following GPC specific items are available:

Command Description

Expand / Collapse Each of the sections can be collapsed or expanded.

Right Click menu

Copy to Clipboard Copies the displayed information AND the calibration data points table to the

Clipboard as a tab separated text.

Export to file… Saves the displayed information AND the calibration data points table to the

file.



6. The GPC Results View

The GPC Results view is accessed from the Results Tab and comprises of the following tabs:

1 Peak Results

2 GPC Column Calibration

3 MW Ranges

4 Percentage Fractions

The Peak Results Tab

This tab consists of a grid containing the calculated MW Averages of the selected processed injection(s).


Alpha The sample Mark-Houwink alpha value.

Data file The filename of the processed injection.

FRCF The flow rate correction factor applied to the processed injection. When the flow

rate correction option is not selected then 1.000 is displayed.

FRM name The flow rate marker name as defined in the processing method being used. When

the flow rate correction option is not selected then this field is blank.

FRM RT (min) The flow rate marker peak retention time (in minutes) of the processed injection.

When the flow rate correction option is not selected then 0.000 is displayed.

K ((10e-5) dL/g) The sample Mark-Houwink K value.

Method The name of the processing method used.



Mn (g/mol) The calculated Number Average (Mn) of the processed peak.

Mp (g/mol) The calculated Peak MW of the processed peak.

Mv (g/mol) The calculated Viscosity Average (Mv) of the processed peak.

Mw (g/mol) The calculated Weight Average (Mw) of the processed peak.

Mz (g/mol) The calculated Mz of the processed peak.

Mz+1 (g/mol) The calculated Mz+1 of the processed peak.

PD The calculated polydispersity (Mw/Mn) of the processed peak.

Peak # The peak number in the injection

Results Set The name of the results set containing the injection.

RT (min) The peak retention time (in minutes) of the processed peak.

Sample name The injection name.

Signal description The processed detector signal of the injection.

Functions available

▪ Order on the active column

▪ Re size the displayed columns

▪ Re order the displayed columns


Command Description

Choose columns … Displays the Choose Columns dialog.

Numeric precision … if relevant, displays the Numeric Precision dialog.

Copy to Clipboard Copies the displayed information and the calibration data points table to the

clipboard as a tab separated text.

Export to file… Saves the displayed information and the calibration data points table to the

file.



The GPC Column Calibration Tab

This tab displays details about the GPC calibration used and how it was derived.

Functions available


Command Description



Export to file… Saves the displayed information and the calibration data points table to the file.

The MW Ranges Tab

This tab displays a table which contains a row for each MW Range defined in the method for each peak in the processed injection.



High limit MW (g/mol) The actual high limit value used for the processed peak.

Low limit MW (g/mol) The actual value of the low limit in the MW Ranges table in the

processing method.


Method high limit MW (g/mol) The high limit value in the MW Ranges table in the processing

method used.

Method low limit MW (g/mol) The value of the low limit in the MW Ranges table in the processing

method.


Percent MW The calculated percentage of the injection of the MW range % .


Sample name The name of the injection.

Signal description The processed detector signal of the injection.



MW Range Name The optional text label defined for a MW Range in the processing

method.

Functions available





Command Description






file.

The Percentage Fractions Tab

This tab displays a table which contains a row for each Percentage Fraction defined in the method for each peak in the processed injection.




MW at high fraction (g/mol) The actual slice MW at the retention time of the high fraction

percentage specified in the method.

MW at low fraction (g/mol) The slice MW at the retention time of the low fraction percentage

specified in the method.

High fraction Mn (g/mol) The calculated Mn average for the high fraction percentage specified

in the method.

High fraction Mw (g/mol) The calculated Mw average for the high fraction percentage specified

in the method.

High fraction percent The high fraction percentage specified in the method.



High fraction RT (min) The actual retention time of the high fraction percentage specified in

the method.

Low fraction Mn (g/mol) The calculated Mn average for the low fraction percentage specified in

the method.

Low fraction Mw (g/mol) The calculated Mw average for the low fraction percentage specified in

the method.

Low fraction percent The low fraction percentage specified in the method.

Low fraction RT (min) The actual retention time at the low fraction percentage specified in

the method.



Sample name The name of the injection.

Signal description The processed signal of the injection.

Functions available





Command Description






file.

The GPC Distributions View


7. The GPC Distributions View

The GPC Distributions view is accessed from the Results Tab and comprises of a read only plot of the GPC molecular weight distribution plot(s) for the selected processed injection(s).

If the processed injection contains more than one processed peak, all distribution plots are displayed in the same color on the same plot.

If more than one processed injection is selected, the distribution plots of all injections are displayed on the same plot. The processed injections can be from the same or different results sets.

Content

Plot Contents Plot of dw/dlogM -v- Log MW

The Cumulative Ht (%) is plotted on the 2nd Y axis

This plot can be selected by the button on the plot window

The color of the plot is linked to the color of the source injection

Y1 Axis scale Linear Y1 Axis units Y1 Axis title dw/dLogM

Y2 Axis scale Linear Y2 Axis units Y2 Axis title Ht (%)

X Axis scale Log X Axis units 1 ex X Axis title Fitted MW (g/mol)

Legend Displays the injection name and filename of the source injection(s)

The GPC Distributions View


Functions available


Button Function

Display the Distribution plot(s).

Display the Distribution plot(s) and associated cumulative plot(s).

Auto scales the plot.

Command Description

Zoom The ability to zoom in on the graph by drawing a box using the mouse

cursor.


Auto Scale Autoscales the plot

Copy to clipboard Copies the plot as EMF (vector) format.

Export to file Displays the standard OpenLab ‘Save As’ dialog.



8. The GPC Calibrations Plot View

The GPC Calibration Plot view is accessed from the Results Tab and comprises of a read only plot of the column calibration plot(s) for the selected processed injection(s).

If more than one processed injection is selected, the column calibration plot(s) are overlaid on the same plot.

The processed injections can be from the same or different results sets.

Content

Plot Contents Plot of Log MW -v- RT corrected (min)

Which contains the data points and calculated line of fit

The color of the line is linked to the color of the source injection

Y Axis scale Log MW Y Axis units 1 ex Y Axis title MW (g/mol)

X Axis scale Linear X Axis units Minutes X Axis title Retention time (min)

Legend Displays the sample name and filename of the injection analysed by the calibration.



Functions available


Command Description

Zoom The ability to zoom in on the graph by drawing a box using the mouse

cursor.

Tooltip When the mouse cursor is over a data point in the calibration plot, a tool

tip displays the following information:

• The retention time (min) of the data point.

• The MW (g/mol) assigned to the data point.

• The sample name of the source chromatogram.

• The filename of the source chromatogram.

The values are taken from the GPC column calibration used to process the

sample of the selected (active) injection.

The ‘Retention Time’ value displayed is the value displayed in the ‘RT

corrected’ column of the GPC Calibration Points tab of the method.


Auto Scale Autoscales the plot

Copy to clipboard Copies the plot as EMF (vector) format.

Export to file Displays the standard OpenLab ‘Save As’ dialog.

Reporting


9. Reporting

The OpenLab Reporting tool can be used to generate reports and also define and modify your own report templates. It is accessed from the Reporting navigation option.

Familiarization with Reporting

Full information about the features and options available are described in the OpenLab Help & Learning tool.

Home > How To > Reporting

The section covers:

▪ Viewing existing reports

▪ Creating injection reports manually in Data Analysis

▪ Creating injection reports automatically after acquisition

▪ Creating a result set summary report

▪ Previewing a new report

▪ Printing a report from the preview

▪ Saving a report from the preview

▪ Specifying PDF options

▪ Selecting a printer

▪ Specifying a fixed scaling for reports

Reporting


Report Types and Generation of Reports

There are three main report types available:

▪ Single Injection

▪ Single Sequence Summary

▪ Cross Sequence Summary

Single injection reports can be generated:

▪ Unattended, by define reporting in the acquisition method

▪ Automatically, by define reporting in processing method

▪ Manually, using the Reporting View

Sequence Summary and Cross Sequence Summary reports are generated interactively from within the Reporting View. The following section provides a summary of the interaction between report types, report items and the injections selected.

Using a Single Injection Report Type

Single Injection Selected

This will produce a single

report for the selected

injection

Series of Injections selected in a single sequence.

This will produce a separate

report for each of the

selected injections

Reporting


Using a Single Sequence Summary Report Type

Series of injections selected in a single sequence.


report with each of the

selected injections overlaid

and combined into one report.

Series of Selected Injections Across Sequences

This will produce a separate

report for each of the

sequences combining the

selected injections per

sequence.

Using a Cross Sequence Summary Report Type

Series of Injections selected Across Sequences


report with all selected

injections from all sequences

overlaid and combined in one

report.

Reporting


Reports Items

The GPC/SEC software provides GPC Specific report items that comprise of a series of GPC specific tables and plots which can be included into the standard OpenLab reports. These are described in the next section.

Example GPC & SEC Report Templates.

Two sets of default report templates are supplied, one set for typical GPC applications and the second for SEC applications.

Further information on the names and content of the supplied reports is provided in the Appendix.

Reporting


GPC additions to the OpenLab Reporting module

The following section describes the GPC additions to the OpenLab Reporting module.

▪ Additions to existing report Items

▪ Addition of GPC specific report items

▪ GPC column calibration specific items

▪ GPC analysis specific items

Additions to Existing Report Items

The following report items are updated to provide ‘GPC’ specific information to the following ‘Data Analysis Method Information’ report items:

Data Analysis Method Information Multi Column

Single Data Analysis Method Parameter

Single Data Analysis Method Table Row

The Data Analysis Method Information Multi Column Item

The following GPC specific parameters are output at the end of the Data Analysis method report.

GPC Method Parameters

MW Ranges Table

Percentage Fractions Table


GPC Calibration Data Points Table

Peak Identification Table (Narrow Standard calibration)

Broad Hamielec Parameters (Broad Hamielec calibration)

Broad Integrals Table (Broad Integral calibration)

The Single Data Analysis Method Parameter Item

This report item allows the selection of a single parameter for display.

Reporting


The following sections are added to this item.

Method Parameters



The Single Data Analysis Method Table Row Item

This report item allows the selection of a single table row for display. The following sections are added to this item.

Method Parameters



Reporting


GPC Specific Report Items

GPC specific report items are provided which comprise of a series of tables and plots. The GPC report items can be found in the GPC node in the Reporting View under ‘Report Items’.

The added items can be divided into:

GPC Column Calibration Specific Items GPC Analysis Specific Items

GPC Column Calibration Details Table Peak Results Table

GPC Calibration Points Table Peak Results Summary Table

Single GPC Calibration Plot MW Ranges Table

GPC Calibration Plot Overlaid MW Ranges Summary Table

Percentage Fractions Table

Percentage Fractions Summary Table

GPC Time Slice Table

Single GPC Distribution Plot

GPC Distribution Plot Overlaid

Reporting


GPC Column Calibration Specific Items

The GPC Column Calibration Details Table Item

Provides a two-column table (<parameter name>, <value>) which provides the following information:

Method name Residual sum of squares FRM RT (min)

Calibration type Coefficient of determination FRM source

Signal Linear correlation coefficient High MW limit RT (min)

K ((10e-5) dL/g) Corrected sum of squares Low MW limit RT (min)

Alpha Standard Y error estimate High limit MW (g/mol)

Order of curve fit FRM name Low limit MW (g/mol)

Curve fit equation

Customization Available

The items and the order in which they are displayed are fixed. The format of individual items in the table cannot be customized.

The GPC Calibration Points Table Item

Provides the following parameters for each calibration data point:

RT corrected (min) Sample name Residual

RT actual (min) Source chromatogram Source chromatogram data

sequence

Source chromatogram project Predicted MW (g/mol) Assigned MW (g/mol)

Signal FRM RT (min) Log MW

Percent error


The items and the order in which they are displayed can be changed. The properties of each parameter column can be customized.

Reporting


The Single GPC Calibration Plot Item

Provides a GPC Calibration Plot which contains a plot of Log MW (g/mol) vs Retention Time (min).

If this item is used in a Single Injection report, the output will consist of a plot of the GPC calibration used to process the injection.

If this item is used in a Sequence Summary report, the output will consist of a separate calibration plot, one for each injection in the sequence summary.


Plot Properties

Show gridlines checkbox If checked, the axes gridlines are displayed

on the calibration plot

Show legend checkbox If checked, the name of the injection is

displayed on the top left corner of the plot

Show calibration points checkbox If checked, the individual calibration data

points are displayed in the calibration plot

The following items allow you to define:

Color of points The color of the calibration data points

Point size The point size of the calibration data points

Point shape The point shape of the calibration data

points

Show calibration line checkbox If checked, displays the calculated line of fit

in the calibration plot


Line color The color of the calibration line

Line weight The thickness of the calibration line

Reporting


The options available in this dialog allow you to define the axes limits for the GPC Calibration plot item.

Plot Scaling

MW Axis custom scaling checkbox MW Axis custom scaling checkbox

Minimum & Maximum limits Minimum & Maximum limits

RT axis custom scaling checkbox RT axis custom scaling checkbox


The GPC Calibration Plot Overlaid Item

Provides a GPC Calibration Plot which contains overlaid plots of Log MW (g/mol) vs Retention Time (min).

If this item is used in a Single Injection report, the output will consist of a single plot of the GPC calibration used to process the injection.

If this item is used in a Sequence Summary report, the output will consist of a single plot contain an overlay of all the GPC calibrations, one from each selected injection in the sequence summary.


Plot Properties

Show gridlines checkbox If checked, the axes gridlines are displayed on the

calibration plot

Injection Colors The color of the calibration line and the data points

can be defined for each individual injection # (1- 8).

Show calibration points checkbox If checked, the individual calibration data points will

be displayed in the calibration plot

The following items allow you to select:

Point size The point size of the calibration data points

Point shape The point shape of the calibration data points

Show calibration line checkbox If checked, displays the calculated line of fit in the

calibration plot

Show calibration line checkbox

Line weight The thickness of the calibration line can be defined

The options available in this dialog allow you to define the axes limits for the GPC Calibration plot item.

Reporting


Plot Scaling

MW Axis custom scaling checkbox MW Axis custom scaling checkbox


RT axis custom scaling checkbox RT axis custom scaling checkbox


GPC Analysis Specific Items

The Peak Results Table Items

Both tables provide the following parameters for each processed peak:

Peak# Mp (g/mol) PD

Sample name Mn (g/mol) FRM name

Data file Mw (g/mol) FRM RT (min)

Signal description Mz (g/mol) FRCF

Method Mz+1 (g/mol) K ((10e-5) dL/g)

Results set Mv (g/mol) Alpha

RT (min)

The Peak Results Table Item

If this item is used in a Single Injection report, the output will consist of a table containing the calculated MW Averages for the selected processed injection.

If this item is used in a Sequence Summary report, the output will consist of a separate table containing the calculated MW Averages, one table for each selected injection in the sequence summary.

The Peak Results Summary Table Item

If this item is used in a Single Injection report, the output will consist of a table containing the calculated MW Averages for the selected processed injection.

If this item is used in a Sequence Summary report, the output will consist of a single table containing the calculated MW Averages for all selected injections in the sequence summary.

Reporting



The items displayed and the order in which they are displayed can be changed. The properties of each parameter column can be customised.

The MW Ranges Table Items

Both tables provide the following parameters for each processed peak:

Peak# Method Method low limit MW (g/mol)

Sample name Results set Low limit MW (g/mol)

Data file Method high limit MW (g/mol) Percent MW

Signal description High limit MW (g/mol) MW Range Name

The MW Ranges Table Item

If this item is used in a Single Injection report, the output will consist of table containing the calculated MW ranges for the selected processed injection.

If this item is used in a Sequence Summary report, the output will consist of a separate table containing the calculated MW ranges, one table for each selected injection in the sequence summary.

The MW Ranges Summary Table Item

If this item is used in a Single Injection report, the output will consist of a table containing the calculated MW ranges for the selected processed injection.

If this item is used in a Sequence Summary report, the output will consist of a single table containing the calculated MW Ranges for all selected injections in the sequence summary.


The items displayed and the order in which they are displayed can be changed. The properties of each parameter column can be customized.

Reporting


The Percentage Fractions Table Items

Both items provide the following parameters for each processed peak:

Peak# High fraction percent Low fraction percent

Sample name High fraction RT [min) Low fraction RT (min)

Data file MW at high fraction (g/mol) MW at low fraction (g/mol)

Signal description High fraction Mn (g/mol) Low fraction Mn (g/mol)

Method High fraction Mw (g/mol) Low fraction Mw (g/mol)

Results set

The Percentage Fractions Table Item

If this item is used in a Single Injection report, the output will consist of a table containing the calculated Percentage Fractions for the selected processed injection.

If this item is used in a Sequence Summary report, the output will consist of a separate table containing the calculated Percentage Fractions, one table for each selected injection in the sequence summary.

The Percentage Fractions Summary Table Item

If this item is used in a Single Injection report, the output will consist of a table containing the calculated Percentage Fractions for the selected processed injection.

If this item is used in a Sequence Summary report, the output will consist of a single table containing the calculated Percentage Fractions for all selected injections in the sequence summary.



Reporting


The GPC Time Slice Table Items

This item provides the following parameters for each processed peak:

Peak# RT (min) dw/dLogM

Sample name Response Cum Ht

Data file Slice MW Norm Ht

Signal description LogM

Method

Results set

If this item is used in a Single Injection report, the output will consist of a table containing the GPC time slice values for the selected processed injection(s).



The Single GPC Distribution Plot Item

Provides a GPC Distribution Plot which contains a plot of

▪ dw/dLogM vs Fitted MW (g/mol)

▪ Ht (%) vs Fitted MW (g/mol)

If this item, is used in a Single Injection report;

▪ Each distribution plot from an injection will be displayed on a separate plot in the report.

If this item, is used in a Sequence Summary report;

▪ Each distribution plot from an injection will be displayed on a separate plot in the report.


Plot Properties

Show gridlines checkbox If checked, the axes gridlines are displayed on the GPC

Distribution plot

Show legend checkbox If checked, the name of the injection is displayed on the top

left corner of the plot

Reporting


Distribution


Line Color The color of the GPC Distribution plot

Line weight The thickness of the GPC Distribution plot

Show Cumulative plot checkbox If checked, displays the Cumulative plot on the second Y

axis.


Line Color The color of the Cumulative plot

Line weight The thickness of the Cumulative plot

Plot Scaling

MW Axis custom scaling checkbox (X axis)

Minimum limits (g/mol or Daltons)

Maximum limits (g/mol or Daltons)

dw/dlogM axis custom scaling checkbox (Y1 axis)

Minimum dw/dlogM Axis limit

Maximum dw/dlogM Axis limit

Percentage height axis custom scaling checkbox (Y2 axis)

Minimum Percentage height axis limit (%)

Maximum Percentage height axis limit (%)

The GPC Distribution Plot Overlaid Item

Provides a GPC Distribution Plot Overlaid which contains overlaid plots of

▪ dw/dLogM vs Fitted MW (g/mol)

▪ Ht (%) vs Fitted MW (g/mol)

If this item, is used in a Single Injection report;

▪ All the distribution plots from an injection will be displayed on one plot on the report.

If this item, is used in a Sequence Summary report:

▪ All the distribution plots from all injections will be displayed on one plot on the report.

Reporting



Plot Properties

Show gridlines checkbox If checked, the axes gridlines are displayed on the GPC

Distribution plot

Show legend checkbox If checked, the name of the injection is displayed on the top

left corner of the plot

Injection Colors The color of the GPC Distribution plot (and cumulative plot

is selected) can be defined for each individual injection #

(1- 8).

Distribution

Line weight The thickness of the GPC Distribution plot

Show Cumulative plot checkbox If checked, displays the Cumulative plot on the second Y

axis.

Line weight The thickness of the Cumulative plot

Reporting


Plot Scaling

MW Axis custom scaling checkbox (X axis)

Minimum limits (g/mol or Daltons)

Maximum limits (g/mol or Daltons)

dw/dlogM axis custom scaling checkbox (Y1 axis)

Minimum dw/dlogM Axis limit

Maximum dw/dlogM Axis limit

Percentage height axis custom scaling checkbox (Y2 axis)

Minimum Percentage height axis limit (%)

Maximum Percentage height axis limit (%)

The following table outlines the GPC Report items and their use in the three different report types

Report Type

Injection Sequence Cross Sequence

GPC Column Calibration Specific Items

GPC Column Calibration Details Table Y

GPC Calibration Points Table Y

Single GPC Calibration Plot Y

GPC Calibration Plot Overlaid Y Y Y

GPC Analysis Specific Items

Peak Results Table Y

Peak Results Summary Table Y Y

MW Ranges Table Y

MW Ranges Summary Table Y Y

Percentage Fractions Table Y

Percentage Fractions Summary Table Y Y

GPC Time Slice Table Y

Single GPC Distribution Plot Y

GPC Distribution Plot Overlaid Y Y Y

Reporting


Report Type Selection Guide

If you require:

A detailed report per injection.

Use the Report Type: Injection Report

GPC Report item type:

A single report that provides a summary for the selected injections in a sequence in a project.

Use the Report Type: Single Sequence Summary

GPC Report item type: Use the summary table and overlaid plot versions of GPC

report items

A single report that provides a summary for the selected injections across a number of sequences in a project.

Use the Report Type: Cross Sequence Summary

GPC Report item type: Use the summary table and overlaid plot versions of GPC

report items

Reporting



Compliance


10. Compliance

Storage of Parameters and Results

The GPC specific processing parameters, column calibrations, GPC results and report templates are all stored within the OpenLab CDS system.

▪ The GPC specific processing parameters and column calibration are stored as part of the processing method

▪ The GPC results generated from an injection are stored as part of the results of a processed Injection

GPC Specific Privileges & Roles

The GPC/SEC software uses the compliance, roles and privileges features provided by OpenLab Control Panel/Shared Services and provides three GPC specific privileges:

GPC specific privileges Location

Ability to edit GPC Parameters in a processing method Project / Processing Method / Edit GPC parameters

Ability to create and modify a GPC column calibration Project / Create and modify GPC calibration

Ability to perform a GPC analysis Project / Data Processing / Do GPC analysis

Compliance


The GPC specific privileges are assigned to the following default roles provided within the OpenLab CDS platform.

GPC Privileges

Role Edit GPC

parameters

Create and modify

GPC calibration Do GPC analysis

Everything Y Y Y

Chemist Y Y Y

Technician N N Y

These privileges mean that a user assigned as:

A Chemist is able to:

Define/edit a processing method for

GPC

Generate/modify a GPC column

calibration

Generate GPC results of samples

A Technician is only able to:

Generate GPC results of samples

The ability to edit GPC processing

parameters and create a GPC

calibration are locked out

Auditing

The GPC/SEC software hooks into the following OpenLab audit processes:

1 The processing method audit trail

2 The injection audit trail

3 The result set audit trail

Logs

The GPC/SEC software log is accessible from the Diagnostics/Logs section.

Format of the Log

The log file uses the same format as the other OpenLab log files.

Content of the Log

The content uses the same format as the other OpenLab log files.

Compliance


Diagnostics

General

Diagnostic information about the GPC/SEC software is accessible from the Diagnostics section of the Administration section accessed from the OpenLab Control Panel.

Installed Components

No GPC specific information is shown in this area.

Compliance



Exporting Information


11. Exporting Information

The standard export features provided by OpenLab are available within the various GPC specific windows and grids, allowing:

Graphics (Chromatograms, calibrations & distribution plots) to be exported to the standard graphic formats (EMF (*.emf) and PNG (*.png)).

The contents of tables and grids to be exported to various standard file formats. (CSV File (*.csv), Excel Workbook (*.xls), Word document (*.doc) and PDF File (*.pdf))

In addition, an option is available which allows the GPC results of a processed injection to be exported as a simple ASCII file. The generated ASCII file can be loaded directly into Excel and provides access to the full GPC results and slice by slice data of the processed peak(s) within the injection.

Processing Method

The parameters defined in a processing method can be exported to the standard file formats using a suitable report template containing the Data Analysis Method Information Multi Column report item accessed from the Method Information section.




Column Calibration Plot

The Column calibration plot can be exported as a graphic image from the GPC Calibration Plot tab of the processing method using the options on the right click menu available in the tab.

Column Calibration Data Points & Details

The GPC column calibration data points table can be exported to the standard file formats using the options on the right click menu available in the GPC Calibration Plot tab of the processing method.

The GPC Column Calibration data points table and the calibration details can be exported to the standard file formats using the options on the right click menu available in the right click menu available in the GPC Calibration Details tab.

GPC Results

MW Averages

The MW Averages and related information displayed in the Peak Results Tab of the GPC Results Window accessed from the Results View can be exported to the standard file formats using the options on the right click menu available in the Peak Results tab.

MW Ranges

The MW Ranges table displayed in the MW Ranges Tab of the GPC Results Window accessed from the Results View can be exported to the standard file formats using the options on the right click menu available in the MW Ranges tab.




The Percentage Fractions table displayed in the Percentage Fractions tab of the GPC Results Window accessed from the Results View can be exported to the standard file formats using the options on the right click menu available in the Percentage Fractions tab.

Full GPC Results and Slice Table

The full GPC analysis results including the peak slice table can be exported as a tab separated ASCII text.

Click on the GPC Results Window to enable the GPC Results menu on the ribbon bar.

Click on this menu item and select the Export Results option which will display the Save as dialog.

MW Distribution & Cumulative Plots

The Distribution & Cumulative Plots displayed in the GPC Distributions window accessed from the Results View can be exported as a graphic image using the options on the right click menu available in the GPC Distributions window.

Column Calibration Used to Process an injection

▪ The Column Calibration plot displayed in the GPC Calibration Plot View

accessed from the Results View can be exported as a graphic image using the options on the right click menu available in the GPC Calibration Plot View.

▪ The GPC Column Calibration data points table and the calibration details can be exported to text from the GPC Column Calibration tab in the GPC Results view accessed from the Results View by using the options on the right click menu available in the GPC Column Calibration tab.

Appendix


12. Appendix

Licensing

A GPC specific data analysis license is delivered as part of the GPC Data Analysis software.

▪ There is no GPC specific ‘Data Acquisition’ license

▪ The GPC/SEC software does not restrict the number of GPC instruments that can be configured on a system

▪ The GPC license is provided in the standard 60 day startup license

▪ The GPC license is installed through the OpenLab Control Panel

Configurations

Workstation Installation

Any concurrent instances of Data Analysis will have the ability to use the GPC module. All concurrent instances of Data Analysis running on the PC will have the ability to use the GPC module.

Client/Server Installation

This configuration provides a pool of GPC analysis licenses available from the server on a “first come first served” basis. The number of concurrent seats possible is by the GPC analysis license file installed.

Appendix


AIC Installation

In order to perform unattended automatic GPC processing, any AIC to be used for GPC applications requires the GPC software installing on the AIC and a GPC license.

License Enforcing

The GPC analysis license only protects the GPC processing functionality within OpenLab Data Analysis. The PC can be used to process data using other processing method types.

Instrument control and data acquisition using OpenLab is not protected by the GPC analysis license.

The generation of report templates and reports is not protected by the GPC analysis license.

GPC Analysis License Available

The following GPC functions and features are available when a project is loaded into an instance of Data Analysis.

GPC/SEC Processing Method

• Creating a new GPC method

• Modifying an existing GPC method


• Processing injections using a GPC method to generate a GPC column calibration for the method

• Reviewing an existing GPC column calibration associated with a GPC method

GPC Analysis

• Processing unprocessed injections using a GPC method to generate new GPC results.

• Reprocessing injections using a GPC method to generate new GPC results.

• Reviewing existing GPC results of processed injections.

Appendix


GPC Analysis License Not Available

If a GPC License is not available (not installed or no license available), then the user will not be able to perform GPC processing, the GPC/SEC software will function only as a ‘GPC Results Reviewer’.

The following GPC functions will not be available when a project is loaded into an instance of Data Analysis and no GPC license is available.

GPC/SEC Processing Method

The GPC parts of a processing method are locked.

1 A user can edit an existing processing method or create a new processing method or of any other type.

2 If a user loads an existing processing method or creates a new processing method (Method type = ‘GPC’) then the following error message is displayed. “Error Agilent GPC Analysis license is not available. GPC processing is disabled” The processing method will still be loaded or created.

For Cases 1 & 2 above:

1 All the GPC processing parameters and any associated GPC column calibration will be viewable in the ‘GPC/GPC Method’ and ‘GPC/GPC Column Calibration’ sections of the processing method.

2 It is still possible to edit generic parts of the processing method but the warning “inconsistency between results and parameters (method or injection list) – reprocess to resolve” will be displayed.

Appendix


GPC Column Calibration Functions

The user will be able to view an existing GPC column calibration associated with a GPC processing method.

The user will NOT be able to process injections to generate a GPC column calibration for a GPC processing method.

GPC Analysis Functions

Existing GPC Results

The GPC results of any processed injections will be viewable but will be locked as read only.

Processing/Reprocessing Injections

The user will not be able to create new GPC results from injections. (e.g. manually changing integration limits, processing an injection or reprocess an injection.) On reprocessing injections (either to generate a column calibration or process an injection), the following error will be displayed.

Injection processed (with errors) Errors: GPC Analysis: No GPC analysis license is available

No results will be generated and any existing GPC results will be cleared for the instance of the analysis session.

▪ The content of all tabs in the GPC Results window will be empty. (Peak Results, GPC Column Calibration, MW Ranges and Percentage Fractions)

▪ The GPC MW Distributions window will be empty

▪ The GPC Column Calibrations window will be empty

The user is not able to save the changes so can only exit the results set/project and the existing results will remain unchanged.

Appendix


Loading a Project/Results Set - No GPC Data in the Results Set

If a results set is loaded that does not contain any GPC analyses, (GPC processing method, calibration, injections processed by a GPC method), then no errors or warnings are displayed. It will be possible to process the data using a processing method other than a GPC processing method.

Loading a Project/Results Set - GPC Data in the Data Set

If a results set is loaded that contains GPC analyses, (GPC processing method, column calibration, processed injections), then the following error message is displayed: “Error Agilent GPC Analysis license is not available. GPC processing is disabled”

It is only possible to view existing GPC data and results.

Appendix


The Default Report Templates supplied.

A series of report templates that are specific to GPC and SEC applications are installed as part of the product installation. The report templates are installed to the central location for default report templates.

The report templates consist of two sets, one designed for typical GPC applications and the other for SEC applications.

Each template set is supplied in A4 and Letter paper sizes

The filenames of the template in the two sets supplied are:

GPC Report Type Template Filename

Sample Analysis Injection

Concise Provides details on a per sample injection

basis

GPC_Sample_Analysis

GPC_Sample_Analysis_Letter

Full GPC_Sample_AnalysisLong

GPC_Sample_AnalysisLong_Letter

Sequence Summary

Concise Provides summary reports for a series of

injections in the same sequence

GPC_SeqSummary

GPC_SeqSummary_Letter

Full GPC_SeqSummaryLong

GPC_SeqSummaryLong_Letter

Cross Sequence Summary

Concise Provides summary reports for a series of

injections across sequences

GPC_CrossSeqSummary

GPC_CrossSeqSummary_Letter

Full GPC_CrossSeqSummaryLong

GPC_CrossSeqSummaryLong_Letter

Column Calibration Report

Provides the column calibration used for

the selected injection

GPC_Calibration

GPC_Calibration_Letter

Appendix


SEC Report Type Template Filename

Sample Analysis Injection Provides details on a per sample

injection basis

SEC_Sample_Analysis

SEC_Sample_Analysis_Letter

Sequence Summary Provides a summary report for a series

of injections in the same sequence

SEC_SeqSummary

SEC_SeqSummary_Letter

Cross Sequence Summary Provides a summary report for a series

of injections across sequences

SEC_CrossSeqSummary

SEC_CrossSeqSummary_Letter

Column Calibration Report Provides the column calibration used for

the selected injection

SEC_Calibration

SEC_Calibration_Letter

Appendix


Additions to the OpenLab Platform

GPC Specific Processing

Method Type

A "GPC specific" processing method type is added to the method

options. The GPC method is based on the standard GC/LC Area

Percent method template provided by OpenLab.

GPC Processing

Parameters

The GPC specific processing parameters are accessed from a “GPC

specific” section of the method.

Storage of GPC

Parameters

The GPC specific processing parameters are stored as part of the

method.

Storage of GPC Column

Calibration

A GPC column calibration generated from injections is stored as part

of the method used. Only one GPC column calibration can exist for

the method.

Storage of GPC Results The GPC results generated from an injection are stored as part of the

standard results of the processed injection.

Addition of a GPC Results

View

This view comprises of the following tabs:

Peak Results


MW Ranges


Addition of a GPC

Distributions Plot View

This view comprises of a plot of the GPC Molecular weight

distribution plot(s) for the selected processed Injection(s).

Addition of a GPC

Calibrations Plot View

This view comprises of a plot of the column calibration plot(s) for the

selected processed Injections.

Reporting Additions of GPC specific information to the processing method report

items

Additions of GPC specific report Items.

Appendix


A series of report templates are supplied with the software which

have been designed to cater for the common types of output required

from the software.

Compliance Features Audit logs

Privileges

Standard Functions & Options available

The standard features provided by OpenLab are available within the GPC specific windows and grids.

Graphics

Zoom

Last Zoom

Auto Scale

Copy to Clipboard

Export to file

Grids / Text

Ability to:

Order on the active column

Re size the displayed columns

Re order the displayed columns

Content Specific Right Click Menu

For example:

Choose Column

Numeric Precision

Copy to Clipboard

Export to File

‘Save As’ dialog

Displays the standard OpenLab ‘Save As’

dialog.

Standard available types dependent of the

type of data to be saved.

Appendix


In This Book

This document describes the features and evaluation parameters of the Agilent Technologies GPC/SEC software for the OpenLab CDS platform. It contains the following information:

• Overview

• Getting Started

• Workflows

• The GPC/SEC Processing Method

• The GPC Results View

• The GPC Distributions View

• The GPC Calibrations Plot View

• Reporting

• Compliance

• Exporting Information

• Appendix

© Agilent Technologies 2019

Printed in Germany

08/2019

D0000361

gpc/sec software for openlab cds

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