NATIONAL PHYSICAL LABORATORY

INDUSTRIAL ADVISORY GROUP MEETING ON

MEASUREMENT METHODS RELATED TO

THE CHARACTERISATION AND PROCESSING PROPERTIES OF POLYMERIC MATERIALS

Minutes of the 10th Industrial Advisory Group (IAG) Meeting

held at the National Physical Laboratory, Teddington

Wednesday 18 April 2007

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Participants:

Paul MorrellAWE

Daljit OhbiBespak

Adrian KellyBradford University

Barry HennesseyFord

Barry HaworthLoughborough University

Sue PantenyMaterials in Transport

Mark HolmesPERA

Richard HolmanPaint Research Association

Peter CoxPeter Cox Associates

Alec BarronRailko Ltd

Crispin AllenNPL

Angela DawsonNPL

Bruce DuncanNPL

Martin RidesNPL

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Apologies for absence were received from:

Brian PowellAlpha Technologies Uk

Julian CubittAnglian Windows Ltd

Tol PurewalBespak

Roy CarterCelsum Technologies Ltd

Sarab SahiCereals Processing & Bakery Science

Dilwyn JonesEmral Ltd

John ColbertFaraday Plastics

Mark EdwardsGammadot

Patrick LeeversImperial College

Bill MeredithICI Plc

Ian RobinsonLucite International

David BartonLeeds University

Chris StevensNGF

Paul HolmesPilkington Group Ltd

Alan GeorgePorpoise Viscometers Ltd

Keith SmalleyRoss Ceramics

John DawsonSerco Assurance

Holger NorenbergTechnolox

Steve LackovicWallace Instruments

CONTENTS

1.INTRODUCTION AND MINUTES OF THE PREVIOUS MEETING

2.CHARACTERISATION OF THE FLOW PROPERTIES OF FILLED MATERIALS AND UPDATE ON STANDARDS (H4 & U4)

3.PERFORMANCE PROGRAMME

4.MATERIALS 2007+ PROGRAMME

5.MEASUREMENT METHODS FOR HEAT TRANSFER PROPERTIES DATA FOR APPLICATION TO POLYMERS (H1) AND UPDATE ON STANDARDS (H1)

6.MATERIALS & THERMAL METROLOGY PROGRAMME 2008+

7.MEASUREMENTS FOR THE PREDICTION OF PERCEIVED PRODUCT QUALITY (MONAT)

8.AOB & DATE OF NEXT IAG MEETING

9.DOCUMENTS AND PRESENTATIONS AVAILABLE

10.ACTION ITEMS

11.DISTRIBUTION

1.INTRODUCTION AND MINUTES OF THE PREVIOUS MEETING

Peter Cox (Peter Cox Associates) welcomed all participants to the Industrial Advisory Group (IAG) Meeting on Industrial Advisory Group Meeting on Measurement Methods Related to the Characterisation and Processing Properties of Polymeric Materials, funded by the DTI NMSD Materials research programmes.

The minutes of the 9th IAG meeting held on 25th October 2006 at the National Space Centre, Leicester (obtainable from using the login: “polyprociag_member” and password: “poly30056”) were accepted as written.

Martin Rides commented that the delegates meeting pack held copies of all presentations and a number of relevant handouts, all of which would be available on the web shortly after the meeting from

using the following username and password

USERNAME: polyprociag_member PASSWORD: poly30056

With reference to Action 1 of those Minutes, Martin Rides reported that the intercomparison had not yet been carried out due to the desire to run it in parallel with the larger international intercomparison being organised by NPL in conjunction with Japan. This Action is continued.

ACTION 1: NPL to initiate an intercomparison on thermal conductivity with Avon Rubber and TARRC. Avon/TARRC to supply materials/samples (Action continued from last meeting).

With reference to Action 2, Martin Rides reported that the draft paper on the intercomparison on slip velocity measurement had been sent to intercomparison participants for comment. The paper was now being revised to take into account the comments received and would be submitted for publication shortly. The revision of the paper had taken into account the confidence levels in the power-law fit parameters to the slip data (Action 3).

Action items 4 and 5 were completed as reported in the previous Minutes.

Slides presented during the introduction

2.CHARACTERISATION OF THE FLOW PROPERTIES OF FILLED MATERIALS AND UPDATE ON STANDARDS (H4 & U4)

Presentation: Flow properties of filled materials and standards update

Presentation: A piezoelectric device for rheological measurement

Poster: Experimental evaluation of a piezoelectric cantilever for characterising the rheological properties of fluids

Martin Rides described the project H4: Flow properties of filled materials (2005-08) in which measurement methods for investigating the mix quality of materials were being investigated. He reported briefly that trends in crystallisation temperature with filler content had been observed and would be investigated further as a possible method, in conjunction with rheometry, for assessing the quality of the dispersion. Discussion concerned the role of size distribution of filler and the effect on thermal conductivity. Martin Rides commented that the latter had not been investigated.

Peter Cox asked about confidentiality of data with respect to case studies. Martin Rides replied that case studies were carried out to demonstrate the industrial suitability and relevance of the measurement methods that have been developed as part of the DTI project. Although it was usually necessary to present data to demonstrate this to UK industry it was not necessary to identify specific materials or processing details thereby protecting confidentially. Materials could be referred to generically, e.g. a filled PP.Confidentiality agreements could be drawn up between NPL and the case study participants to ensure confidentiality of specific information.

Crispin Allen reported on results of testing using a PZT piezoelectric cantilever device for rheological measurements - project “U4: Dynamic properties of solid/liquid materials systems at the nano and micro-scale (2005-08)”. Results obtained using this device showed good correlation when used with Newtonian fluids over a viscosity range of approximately 7 decades, and reasonable correlation of measured behaviour with rheological properties for viscoelastic non-Newtonian Xanthan gums. This demonstrates that the technique has significant potential as an in-process monitor of the rheological behaviour of fluids. Further work would be carried out to investigate in more detail the capability of the instrument and to develop it further for non-Newtonian fluids. Martin Rides commented that a copy of the poster that had been presented at the Fourth Annual European Rheology Conference was included in the meeting delegates pack. Richard Holman said that PRA would be interested in PZT testing of emulsions which degrade in the 20 kHz to 40 kHz range. He also enquired as to what applications the technology had been put into practice. Martin Rides replied that he understood that it had been used in in-situ monitoring of engine oil but did not have details. Interest was expressed in cure monitoring without wires.

Martin Rides reported on the development of a disposable extrusion rheometer that could be used for testing curing systems, and presented results obtained using it including against results obtained by oscillatory rheometry.

Martin Rides then provided an update on progress on rheometry standards, in particular on the development of ISO 1133 MFR/MVR to incorporate moisture sensitive materials as a Part 2 to the standard. He invited all to participate in the intercomparison in support of development of this standard, which NPL was organising. The standard was now at CD ballot. Peter Cox expressed interest in seeing a copy of the draft standard that is likely to be published in 2009. He encouraged all to contribute to the standards making process. Barry Hennessey asked for details of the Standards on moisture testing of materials.

ACTION 2: Martin Rides to send Peter Cox copy of draft standard on MVR testing of moisture sensitive materials.

ACTION 3: Martin Rides to provide Barry Hennessey details on moisture testing of materials.

He then commented on some oscillatory rheometry testing of gel materials that exhibited complex behaviour, thought to be slip arising due to the high water content of the samples.

3.PERFORMANCE PROGRAMME

Presentation: Polymers Performance Overview

Bruce Duncan presented a summary of the work of seven projects of relevance in the Performance Programme which had finished at the end of March 2007.

E1Non-Destructive Adhesion Measurements

F2Sensing the Onset of Damage at Polymer Surfaces Due to Environmental Exposure

F4Accelerated Ageing Protocol For Service in Hostile Conditions

F7Permeation, Absorption and Desorption of Liquids and Gases in Polymer and Multilayer Systems

F9Prediction of the Lifetime of Adhesive JointsUnder Sustained Loading

F10Adhesive Design Toolkit

F12Development of Test Methods for Determining the Criticality of Defects in Composite Materials Systems Under Long-term Loading

The outputs of these projects can be found at the website:

and in particular at:

using the username: PolPerf and the password: FPERF (case sensitive).

Interest was expressed by Richard Holman in the diffusion of chemicals other than water into polymers and polymer films and also, for example, of sun tan creams into paint films that can result in flaking off of the paint..

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ACTION 4: Copy of the paper “Weathering of Recycled Photo-Degraded Polyethylene” by A.S. Maxwell, February 2007 (submitted to Polymer Science and Engineering) to be sent to Alec Barron

4.MATERIALS 2007+ PROGRAMME

Martin Rides briefly described some of the projects in the Materials & Thermal Metrology 2007+. NMSD programme. He commented that projects of potential interest to the IAG were (with project leader and code details given):

Fluid properties for micro-processing– Martin Rides (AM10)

Diagnostics for Measuring and Modelling Dispersion in Nanoparticulate Reinforced Polymers– Bill Broughton (AM11)

Enabling the Next Generation of Structural Health Monitoring: Demonstrator, Validation and Best Practice – Michael Gower (AM14)

•Design Toolkit and Non-Destructive Measurements for Lifetime Management of Composite Structures under Dynamic Multi-Axial Loading Conditions - Bill Broughton (AM17)

Moisture in materials - development of measurement capability – Stephanie Bell (UP10)

In particular, he drew attention to the project on fluid properties for micro-fluidics, dispersion in nanoparticulate-reinforced polymers and on moisture in materials.

Daljit Ohbi expressed interest in very low moisture concentration measurements in materials, which was supported also by Paul Morrell.

He commented that the formulation was a rolling process and recommended that ideas were submitted at any time, rather than waiting for a formal request.

For details of the Materials 2007 programme see:

For details of the Materials 2007+ presentation to the IAG see:

Presentation: Materials and Thermal Metrology Programme 2007+

ACTION 5: Martin Rides to circulate a pdf copy of the Materials 2007+ presentation to IAG attendees as soon as possible.

5.MEASUREMENT METHODS FOR HEAT TRANSFER PROPERTIES DATA FOR APPLICATION TO POLYMERS (H1) AND UPDATE ON STANDARDS (H1)

Presentation: Heat Transfer in Polymers

Martin Rides briefly outlined the objectives of the project. Angela Dawson then described in detail measurements using the heat transfer coefficient (HTC) apparatus to determine the effect of interfaces, including that of an polymer - mould and polymer - air gap - mould on heat transfer. Results indicated that an air gap had the same thermal resistance as that of the polymer layer approximately 6 times thicker. The effect of the thermal resistance of the polymer-mould interface was, in comparison, small being of the order of 0.00037 (m2.K)/W. Further planned work entailed a study of the effect of surface finish on heat transfer at a solid polymer-mould interface and the case study with Cinpres which is being progressed to investigate the effect of air gaps on cooling times in processing.

Presentation: Heat Transfer in Polymers HTC Measurements

Martin Rides then briefly described the standardisation activities that were progressing in ISO, and commented that contributions to the standardisation process by industry were welcome. He invited all to participate in the intercomparison on thermal conductivity that was being carried out in support of the standards activity, the first results of which had now been received.

6.MATERIALS & THERMAL METROLOGY PROGRAMME 2008+

Materials and Themal Metrology 2008

Martin Rides provided a brief overview of the rolling formulation approach to the Materials 2008+ programme, and also presented information on the DTI’s Technology Programme (Spring 2007) indicating current priority areas for DTI R&D funding.

ACTION 6: Martin Rides to circulate a pdf copy of the Materials 2008+ presentation to IAG attendees as soon as possible.

7.MEASUREMENTS FOR THE PREDICTION OF PERCEIVED PRODUCT QUALITY (MONAT)

Martin Rides described the recent and planned work on measurements for the prediction of perceived quality of products, presented some results, and reported on the plan to develop a studio project along this theme. This would enable UK companies to take advantage of the EC Framework Programme (FP6). The MONAT project’s objectives are to:

  • Understand neurological and psychological responses involved in perception of ‘naturalness’
  • Identify relationships between physical properties of material and perceived ‘naturalness’
  • Determine most appropriate physical measures for modelling perception of ‘naturalness’
  • Model relationships between physical attributes, sensory network and higher-level cognitive functions to predict perceived ‘naturalness’

Several handouts detailing the studio project and providing further background were included in the delegates meeting pack. For further information contact Martin Rides.

Measurements for the prediction of perceived product quality

Measurements for the prediction of perceived product quality-project description

Measurements for the prediction of perceived product quality (MONAT)-work plan

MONAT measurement of naturalness

Perception is key

8.AOB & DATE OF NEXT IAG MEETING

There was no other business to discuss.

Peter Cox thanked everyone for attending this IAG meeting and invited all to attend the next one before closing the meeting. However, the proposed date of the next meeting was not suitable for the chairman. It was agreed to change the date of the meeting to avoid a clash.

Details of the next meeting have been set since the meeting. The next IAG meeting will be held on:

Thursday 4 October 2007, at RAPRA, Shawbury (near Shrewsbury), Shropshire

An agenda will be circulated one month prior to the meeting. Details of the meeting will be posted on the website in due course. All are invited.

9.DOCUMENTS AND PRESENTATIONS AVAILABLE

The presentations made and the documents distributed at the meeting are available on the website:

using the following username and password

USERNAME: polyprociag_member PASSWORD: poly30056

10.ACTION ITEMS

ACTION 1: NPL to initiate an intercomparison on thermal conductivity with Avon Rubber and TARRC. Avon/TARRC to supply materials/samples (Action continued from last meeting).

ACTION 2: Martin Rides to send Peter Cox copy of draft standard on MVR testing of moisture sensitive materials.

ACTION 3: Martin Rides to provide Barry Hennessey details on moisture testing of materials.

ACTION 4: Copy of the paper “Weathering of Recycled Photo-Degraded Polyethylene” by A.S. Maxwell, February 2007 (submitted to Polymer Science and Engineering) to be sent to Alec Barron

ACTION 5: Martin Rides to circulate a pdf copy of the Materials 2007+ presentation to IAG attendees as soon as possible.

ACTION 6: Martin Rides to circulate a pdf copy of the Materials 2008+ presentation to IAG attendees as soon as possible.

11.DISTRIBUTION

IAG members and NPL staff (by downloading from the NPL website)


AGENDA

MEASUREMENT METHODS RELATED TO

THE CHARACTERISATION AND PROCESSING PROPERTIES

OF POLYMERIC MATERIALS

Industrial Advisory Group (IAG) Meeting

Wednesday 18 April 2007

at NPL (CS6, Module 16)

Teddington, TW11 0LW

Chairman: Peter Cox, Peter Cox Associates

10-30Welcome and IntroductionsAll

10-40Minutes of the previous meetingPeter Cox

10-50Characterisation of the flow properties of filled materials

and update on standards (H4 & U4)Martin Rides/Crispin Allen

11-30Performance Programme 2004-07Bruce Duncan

12-00Materials 2007+ (2007-10)

AM10 Fluids, AM11 Nanocomposites, AM14 SHM, AM17 Composites design

Martin Rides

12-30LUNCH

13-30Measurement methods for heat transfer properties data for application to

polymers (H1) and update on standardsAngela Dawson, Martin Rides

14-10Materials 2008+ programmePeter Cox / Martin Rides / All

14-40Measurementsfor the prediction of perceived product quality (MONAT)

Martin Rides

14-50Date/venue of next meeting (Proposed 10 Oct 2007 / venue tbc)Peter Cox

14-55AOBPeter Cox

15-00Close

Tea/Coffee will be available before the meeting (from 10.00 am) and after the meeting at 15.00.

Further discussions with NPL experts will be possible after 15.00.

For details of the venue see National Physical Laboratory and how to get there see traveldetails.

Brief description of agenda items / projects to be reported on at the IAG meeting

Characterisation of the flow properties of filled materials (H4 & U4) & update on rheological standards

Reliable characterisation of the rheological behaviour of materials is important for design of new materials and processes, and for quality control. Fillers can have a significant effect on the flow properties of materials and can complicate their reliable measurement. This work focuses on the measurement of filled materials, including nano-fillers, and the use of rheological and thermal techniques for assessing the level of dispersion of those filler in materials – an essential factor in the performance of nano-particulate filled materials. Results on the characterisation of filled materials will be presented. Developments in the use of small-scale rheological measurements using piezoelectric cantilevers will also be presented. A brief update on current activity in ISO on standardisation of rheological testing will be presented, focusing on the development of the melt flow rate test for testing moisture sensitive materials, e.g. PET, PBT, PA. See further details.

Performance Programme (2004-07)

A review of the recent Measurements for Materials Performance programme focusing on projects relevant to polymeric materials will be presented. SeeMeasurements for Materials Performance(Theme F) for further details.

Materials 2007+ (2007-10)

An overview of the Materials 2007+ programme, starting 1 April 2007, will be given. The focus of the presentation will be on projects relevant to polymeric materials, namely: AM10 - Fluid properties for micro-processing; AM11 - Diagnostics for Measuring and Modelling Dispersion in Nanoparticulate Reinforced Polymers; AM14 - Enabling the Next Generation of Structural Health Monitoring: Demonstrator, Validation and Best Practice; and AM17 - Design Toolkit and Non-Destructive Measurements for Lifetime Management of Composite Structures under Dynamic Multi-Axial Loading Conditions.

Measurement methods for heat transfer properties data for application to polymers (H1) and update on standards

Reliable characterisation of the heat transfer properties of materials is essential for accurate process simulation and can play a significant role in materials selection and design. This project focuses on the measurement of the heat transfer behaviour of polymers (thermal conductivity and heat transfer coefficients) relevant to polymer processing (the heat transfer coefficient characterises the interface between, for example, the polymer and the mould in injection moulding). Methods for characterising the thermal conductivity of polymers and heat transfer coefficients relevant to polymer processing and the results obtained will be discussed. An update on current activity on standardisation of thermal conductivity measurements of polymers will also be presented.See for further details.