WHAT IS HOT IN GPC

1

Sue D’Antonio

7.5 mm columns

Agilent GPC/SEC Software

Agilent GPC/SEC

Software Multi-

Detector upgrade

Performance

Current Agilent GPC portfolio

Standard GPC

Triple Detection

Light Scattering

and/or

ViscometryEntry level GPC

4.6mm and 2.1mm columns

7.5 mm columns

Advanced GPC

Micro Refractive

Index Detection

1290 Infinity II 1260 Infinity (II)

High temperature GPC

220

With Optional

Triple Detection

Requires Agilent

Software Multi-

Detector upgrade

Optional Agilent Chemstation

Cirrus GPC Plugin Software

A New High Temperature Instrument Configuration

• Reduce analysis times by minimising system equilibration times and

maximising baseline stability

• Multi-tasking GPC software provides full instrument control and the

ability to process complex data for excellent reproducibility

• Incorporate higher sensitivity detection to aid development and

analysis of new, higher performance polymers

Agilent 1260 Infinity II HTGPC System (G7820B)

What’s new…..

• RoHS Compliant

• Standalone pump, giving increased operation flexibility – isocratic as standard; use with binary and

gradient pumps are now possible

• All new electronics offer improved stability, sensitivity and serviceability.

• Includes Full Instrument Control – Completely Windows 10 compatible

• Smaller footprint – Frees up valuable bench space.

• New HT-ELSD detector – State of the art stable, sensitive concentration detector which can also be

used solvent gradients.

• Flexible solvent and waste management – new instrument removes limitations due to solvent

compartment in the previous model.

Agilent 1260 Infinity II HTGPC System (G7820B)

What’s the same…

• Price – comparable to previous system

• Molecular weight detector options – Both the dual angle light scattering detector and viscometer are

still available for the new instrument, but with simplified, improved fitting kits.

• Autosampler – Dual zone temperature control and 40 vial position carousel retains the excellent

reproducibility.

• Refractive Index Detector – Fitted as standard.

• SP260VS Sample Prep System (220V) – Now RoHS compliant

Instrument Control Software

Functionality Retained – Improved layout means easier to use

Instrument Control

Data Collection

GPC/SEC Calculations

Same look-and-feel as the

OpenLAB CDS

ChemStation for HPLC

Easy to move from one

system to another when

deploying both techniques

Powerful Agilent GPC Software

Performance Specifications

Unit Type Specification

Pump Flow Range 0.1 – 10 mL/min Pump

Flow Rate Reproducibility <0.07%

Oven Temperature Range Ambient to 220°C

Temperature Stability <0.05°C/h

Column Capacity 6 x 30cm columns

Detector Differential Refractometer Deflection

Cell Volume 8 μL

Noise ≤80 μV

Drift ≤10 mV/h

Wavelength 890 nm

Autosampler Carousel Capacity 40 x 2 mL Vials

Injection Volume flushed fixed loop; 5 – 500 μL

Precision ≤1 %

Instrument Control Microprocessor

Instrument Interface Windows 10 Advanced PC control

G7820B Specifications

• Weight : 136 kg (300 lbs)

• Dimensions (w x d x h) : 900 x 530 x 620 mm (35.5 x 21 x 24.5 in)

• Packaged size (w x d x h) : 990 x 750 x 1030 mm (39 x 29.5 x 40.5 in)

• Line voltage : 240 VAC, +/- 10%

• Line frequency : 50 or 60 Hz +/- 5%

• Power consumption : 3300 VA, 2310 W/7900 BTU

• Power consumption : 160 VA Maximum

• Operating temperature : Ambient - 220°C (Ambient -428°F) without DRI

: Ambient - 185°C (ambient -365°F) with DRI

• Humidity : <80%, at 25 - 35°C (77-95°F), non-condensing

• Operating altitude : up to 2000 m (6562 feet)

• Non operating altitude : up to 4600 m (15091ft)

Agilent Material Seminar 2016

July 12/15 2016

High Temperature Evaporative Light Scattering Detection (HT ELSD)

NEW

• New High Performance Nebulizer operates at elevated temperatures

• Ambient to 160C

• Detects Extremely Low

concentrations

• Rapid Equilibration Times

• Excellent Baseline Stability

Using ELSD for High Temperature GPC

Polyolefins typically need to be dissolved in low concentrations

ELSD offers excellent baseline stability and sensitivity

0.05%

200ul

Agilent Material Seminar 2016

July 12/15 2016

Polyethylene

(NBS 1475, 0.025%)

Polypropylene

(0.2%w/v)

Two Examples – PP and PE

Illustrating the excellent

response of the HT ELSD to

Polyolefins.

HT-ELSD has a more linear

response to concentration

than DRI.

No negative peaks to hinder

baseline selection and limits

of integration

A chromatogram

The chromatogram shown below taken for a mixture of polystyrene (PS)

standards in 1,2,4-trichlorobenzene (TCB) at 160°C, shows some of the

main advantages of the ELSD detection:-

Removal of the solvent giving stable baseline and no solvent related

peaks at total permeation

Good linear relationship between the sensitivity and concentration

HT ELSD compared to DRI – PS Standards

• HT ELSD is typically 12x more sensitive than the DRI

• The ELSD accurately maps the concentration of the standards injected whereas the DRI

underestimates the low molecular weight standard due to changes in differential refractive index

(dn/dc)

• The ELSD baseline is stable and clean once the polymer has eluted; no solvent peaks as seen

on the DRI (see highlighted area)

• The peaks obtained on the HT-ELSD are always positive unlike the DRI where the differential

refractive index (dn/dc) determines the peak polarity

• Comparing the new HT-ELSD with the previous model (PL-ELS1000)

marketed by the Polymer Laboratories in the late 90s and early 2000s we find

the following

• The peaks are narrower on the PL-ELS 1000

• The response on the PL-ELS 1000 is non-linear

• The 4th peak is ‘evaporated’ by the high temperatures used in the PL-ELS

1000 (Evaporation temperature was set to 270°C compared to 120°C for the

new HT-ELSD)

• Signal/noise for the HT-ELSD is 4x better than the PL-ELS 1000

Comparing Old and New HT-ELSD

• Polyolefin analysis at temperatures of 160°C and above can prove a challenge.

• One of those challenges is often detection, typically Differential Refractive Index (DRI)

• Achieving baseline stability can often take several hours

• Save time and reduce frustration – HT ELSD takes minutes to equilibrate

Why Choose HT ELSD? – Save Time

An overlay of four chromatograms

after a warm up time of only

twenty minutes

Why Choose HT ELSD? – Accurate Integration

• Baseline noise and drift can make it difficult to decide on limits of peak

integration

•

• HT ELSD evaporates all of the solvent prior to detection – smaller baseline

noise and no drift

• Negative peaks at total permeation are almost always present when using

DRI

Why Choose HT ELSD? – Reproducible Results

HT-ELSD has a more linear response to

concentration than DRI.

Polyethylene (PE-B)

Broad polystyrene sample (PS-B)

PE-B

Why Choose HT ELSD? - UHMWPE

• Very broad distribution

• Low concentrations at both low and high molecular weight

• Low dn/dc (differential refractive index) of the polymer/solvent combination

• Low sample concentration needed to eliminate potential viscosity and

overloading issues

In this case the high sensitivity of ELSD makes the detector ideal for low

dn/dc polymer/solvent combinations and also gives a positive response for all

non-volatile solutes.

Availability of a high temperature ELSD would offer considerable advantages

when looking at such types of polymer. In this presentation we introduce a

new HTELSD in development and evaluate the advantages it will bring to the

analysis of UHMWPE.

Summary

The new HT-ELSD demonstrates some great advantages for use as a concentration

detector for high temperature GPC and the analysis of polyolefin including:-

• Superior sensitivity compared to a DRI, making it preferable for UHMWPE samples

that require very low concentration for dissolution and analysis

• Stable baseline, the removal of solvent peaks, and suitability for high temperature

gradient chromatography

• Improved linearity and integrity in the determination of molecular weights due to the

lower operating temperatures

• Unlike DRI, there is the possibility to run solvent gradients at elevated temperatures.

GPC for OpenLAB CDSAt-a-glance

A modern, compliant, scalable GPC/SEC solution

Provides conventional GPC/SEC functionality

Fully integrates into OpenLAB CDS (v2.2 or above)

Able to process any concentration detector signal collected or imported into OpenLAB CDS

GPC for OpenLAB CDS

Key Features

Processing Method Development

Create / Modify a GPC processing method

GPC Calibration

Generate a new GPC calibrations

Review an existing GPC calibration

GPC Analysis

Generate new GPC results

Review existing GPC results

Generating Reports

Generate a GPC report from results

Processing a Sample – GPC Results

GPC Specific

windows are

provided by the

plugin.

Expression & calculation possibilities

• Custom Calculator results

- All results calculated by the CC can be reported

- Special fields on compound, signal, injection and

sequence level

- CC’s can be used in expressions for filtering,

grouping and sorting

• Embed VB code in templates

• Link a custom assembly (dll) to the report

template for additional results or calculations

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GPC Master Class coming to our town

Week of September 11, 2017 at the

Quantum site in the Woodlands