annex ia - jrp-protocoltera.chem.ut.ee/~ivo/temp/sib64_metefnet/contract...euramet tc-m euramet...

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of 69 SIB64 METefnet Annex Ia v1.0

Annex Ia - JRP-Protocol

Version Date: 28 May 2013

SIB64 METefnet

Metrology for Moisture in Materials

Start date: 01 June 2013

JRP-Coordinator Martti Heinonen

MIKES

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Tefnet ( ) was the goddess of moisture, moist air, dew and rain in Ancient Egyptian religion. She was one of the nine most important deities in Egyptian mythology.

In this JRP, moisture is the target and the improvement of moisture metrology in Europe is the goal of the project. To create a unique acronym, we invoked the name of the goddess, and added a metrology twist.

This is METefnet, the JRP short name for the Metrology for Moisture in Materials endeavour.

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Glossary

AC-CBS Artificial Compressibility Characteristic-Based Split

AFRIMETS Intra-Africa Metrology System - RMO for African countries

APMP Asia Pacific Metrology Programme - RMO for Asia-Pacific countries

BIPM International Bureau for Weights and Measures

CCQM Consultative Committee for Amount of Substance

CCQM IAWG Inorganic Analysis Working Group of CCQM

CCQM OAWG Organic Analysis Working Group of CCQM

CCT Consultative Committee for Thermometry

CCT WG6 CCT Working Group 6: humidity

CIPM International Committee for Weights and Measures

CIPM CC Consultative committee of CIPM

cKF coulometric Karl Fischer titration

CMC Calibration and Measurement Capability

COOMET Eura-Asian Cooperation of NMIs - RMO for Eurasian countries

COOMET TC 1.8 COOMET Technical committee for physical chemistry

COOMET TC 1.12 COOMET Technical committee for reference materials

CRM certified reference material

CT Temperature AFRIMETS AFRIMETS Technical committee for temperature

DI Designated institute appointed to hold specific national standard(s)

EA The European Co-operation for Accreditation

EURAMET European Association of National Metrology Institutes - RMO for European countries

EURAMET TC-M EURAMET Technical Committee of Mass and Related Quantities

EURAMET TC-MC EURAMET Technical Committee of Metrology in Chemistry

EURAMET TC-T EURAMET Technical Committee of Thermometry

EURAMET TC-T/SC Humidity EURAMET TC-T Sub-committee for humidity

GPM General project meeting

ILAC International Laboratory Accreditation Cooperation

IR infrared

LoD mass loss on drying

NIR near infrared

NMI National metrology institute

NMR nuclear magnetic resonance

OIML The International Organisation of Legal Metrology

PMB Project management board

R&D research and development

RF radio frequency

RH/T logger temperature-humidity datalogger

RMO Regional metrology organisation

SRM standard reference material

TGA thermogravimetric analyser

water amount fraction amount of water in a sample divided by the amount of all constituents in the sample

water mass fraction mass of water in a sample divided by the total mass of the sample

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Contents

Section A: Key Data for the JRP ................................................................................................................ 5 A1 JRP SUMMARY DATA .......................................................................................................................... 5 A2 RESOURCE SUMMARY ....................................................................................................................... 6 A3 SUMMARY OF PARTICIPATION IN WORK PACKAGES ................................................................... 6

Section B: Overview of the Research ........................................................................................................ 7 B1 SCIENTIFIC AND/OR TECHNICAL EXCELLENCE ............................................................................. 7

B1.a Summary of the JRP ............................................................................................................... 7 B1.b Need for the project ................................................................................................................ 8 B1.c Progress beyond the state of the art ....................................................................................... 9 B1.d Overview of the scientific and technical objectives ............................................................... 11

B2 RELEVANCE TO THE OBJECTIVES OF THE EMRP ....................................................................... 12 B2.a How the JRP addresses the overall objectives of the EMRP ............................................... 12

B3 POTENTIAL IMPACT THROUGH THE DEVELOPMENT, DISSEMINATION AND USE OF THE PROJECT RESULTS .......................................................................................................................... 13

B3.a Projected impact of the JRP ................................................................................................. 13 B3.b Projected JRP impact on EC Directives, and other relevant standards ............................... 15

B4 THE QUALITY AND EFFICIENCY OF THE IMPLEMENTATION AND MANAGEMENT................... 16 B4.a Overview of the JRP-Consortium and JRP management .................................................... 16

Section C: Detailed Project Plans By Workpackage .............................................................................. 17 C1 WP1: Realisation of moisture units ..................................................................................................... 17

C1.a Description of Work ............................................................................................................... 18 C1.b Labour Resources for WP1 ................................................................................................... 22 C1.c Summary of Deliverables for WP1 ........................................................................................ 22

C2 WP2: Traceability and dissemination .................................................................................................. 23 C2.a Description of Work ............................................................................................................... 25 C2.b Labour Resources for WP 2 .................................................................................................. 28 C2.c Summary of Deliverables for WP 2 ....................................................................................... 28

C3 WP3: Metrological underpinning for moisture ..................................................................................... 30 C3.a Description of Work ............................................................................................................... 31 C3.b Labour Resources for WP3 ................................................................................................... 33 C3.c Summary of Deliverables for WP3 ........................................................................................ 34

C4 WP4: Creating Impact ......................................................................................................................... 35 C4.a Description of Work ............................................................................................................... 35 C4.b Labour Resources for WP4 ................................................................................................... 39 C4.c Summary of Deliverables for WP4 ........................................................................................ 40

C5 WP5: JRP Management and Coordination ......................................................................................... 41 C5.a Description of Work ............................................................................................................... 41 C5.b Labour Resources for WP5 ................................................................................................... 42 C5.c Summary of Deliverables for WP5 ........................................................................................ 42

C6 SUMMARY LIST OF ALL DELIVERABLES ........................................................................................ 44 C7 THE PROJECT TIMESCALE: GANTT CHART .................................................................................. 49

C7.a GANTT chart for WP1 ........................................................................................................... 49 C7.b GANTT chart for WP2 ........................................................................................................... 50 C7.c GANTT chart for WP3 ........................................................................................................... 51 C7.d GANTT chart for WP4 ........................................................................................................... 52 C7.e GANTT chart for WP5 ........................................................................................................... 53

Section D: Risk and Risk Mitigation ........................................................................................................ 54 D1 SCIENTIFIC/TECHNICAL RISKS ....................................................................................................... 54 D2 MANAGEMENT RISKS ....................................................................................................................... 56 D3 ETHICAL ISSUES ............................................................................................................................... 56

Section E: Project Resources and Budget Overview ............................................................................ 57 E1 JRP LABOUR RESOURCES (Person Months) .................................................................................. 57 E2 JRP BUDGET BREAKDOWN ............................................................................................................. 57 E3 RATIONALE FOR NON-LABOUR RESOURCES .............................................................................. 57

Section F: Rationale for the JRP-Consortium ........................................................................................ 59 F1 DESCRIPTION OF EACH JRP-PARTICIPANT (EXCEPT COLLABORATORS), INCLUDING KEY

ROLES AND CONTRIBUTIONS ......................................................................................................... 59

Section G: Collaborators........................................................................................................................... 68

Section H: References ............................................................................................................................... 69

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Section A: Key Data for the JRP

A1 JRP SUMMARY DATA

JRP Title and JRP-Coordinator contact details:

JRP Number SIB64

JRP Short Name METefnet

Full JRP Title Metrology for moisture in materials

Coordinating Organisation

Mittatekniikan Keskus (MIKES)

JRP-Coordinator Martti Heinonen

Address Tekniikantie 1, P.O. Box 9, FI-02151 Espoo, Finland

Phone: +358 29 5054 402

Email: [email protected]

Key Dates:

Start date End date Duration

JRP 1 June 2013 31 May 2016 36 months

REG(UNICLAM) 1 June 2013 31 May 2016 36 months (full time)

JRP-Participant details:

a. JRP-Partners (those who will accede to the JRP-Contract)

no. Participant Type Short Name Organisation legal full name Country

1 Funded JRP-Partner MIKES Mittatekniikan Keskus Finland

2 Funded JRP-Partner BRML Biroul Roman de Metrologie Legala Romania

3 Funded JRP-Partner CETIAT Centre Technique des Industries Aérauliques et Thermiques

France

4 Funded JRP-Partner CMI Cesky Metrologicky Institut Brno Czech Republic

5 Funded JRP-Partner DTI Teknologisk Institut Denmark

6 Funded JRP-Partner INRIM Istituto Nazionale di Ricerca Metrologica Italy

7 Funded JRP-Partner NPL NPL Management Limited United Kingdom

8 Funded JRP-Partner TUBITAK Turkiye Bilimsel ve Teknolojik Arastirma Kurumu

Turkey

9 Funded JRP-Partner UL Univerza v Ljubljani Slovenia

10 Funded JRP-Partner UT Tartu Ülikool Estonia

b. Other JRP-Participants (those who will NOT accede to the JRP-Contract)

no. Participant Type Short Name Organisation legal full name Country

11 Integral REG UNICLAM Università degli Studi di Cassino e del Lazio Meridionale

Italy

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A2 RESOURCE SUMMARY

Financial Resources

Total eligible costs (€)

EURAMET contribution

(€)

Unfunded JRP-Partner contribution

(months)

Integral REG contribution

(months)

2 717 030.11 1 162 888.89 0.0 36.0

Labour Resources (person months)

1- M

IKE

S

2- B

RM

L

3- C

ETIA

T4-

CM

I

5- D

TI

6- IN

RIM

7- N

PL

8- T

UBIT

AK

9- U

L

10- U

T

11- R

EG

(UN

ICLA

M)

TO

TA

L

WP1 14.0 18.0 2.5 13.0 14.5 7.0 28.5 97.5

WP2 7.0 9.5 13.0 10.0 11.0 12.5 7.0 11.6 2.0 83.6

WP3 10.0 7.0 1.0 17.0 6.0 3.5 2.0 33.0 79.5

WP4 2.0 2.0 2.0 2.0 1.8 2.0 4.0 1.7 1.5 3.0 2.0 24.0

WP5 5.0 0.5 1.5 0.5 0.5 1.5 1.5 0.5 0.5 0.5 1.0 13.5

TOTAL 28.0 40.0 19.0 19.5 16.3 31.5 32.5 22.2 17.1 36.0 36.0 298.1

A3 SUMMARY OF PARTICIPATION IN WORK PACKAGES

WP No Work Package Name Active JRP-Participants (WP leader in bold)

WP1 Realisation of moisture units MIKES, DTI, BRML, CETIAT, NPL, TUBITAK, UT

WP2 Traceability and dissemination CETIAT, BRML, CMI, INRIM, MIKES, NPL, UL, TUBITAK, UT

WP3 Metrological underpinning for moisture INRIM, CMI, DTI, BRML, UL, TUBITAK, UT, REG(UNICLAM)

WP4 Creating Impact NPL, BRML, CMI, CETIAT, DTI, INRIM, MIKES, UL, TUBITAK, UT, REG(UNICLAM)

WP5 JRP Management and Coordination MIKES, BRML, CMI, CETIAT, DTI, INRIM, NPL, UL, TUBITAK, UT, REG(UNICLAM)

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Section B: Overview of the Research

B1 SCIENTIFIC AND/OR TECHNICAL EXCELLENCE

B1.a Summary of the JRP

Active ingredients in pharmaceuticals, carbon-fibre composites, polymers, novel cellulose-based active paper, food powders, biomass – all of these and many other solid materials are highly affected by moisture when processing into various products. Errors and inconsistencies in moisture measurement and control in industrial processes lead to decreased process speed/throughput and increased wastage, shortened durability of biomaterials, increased energy consumption in drying and increased fine particle emissions in biomass combustion. More than 1300 documentary standards are in active use because available measurement methods, reference methods and even the current definitions for moisture as a measurand are material specific.

The quality of moisture measurements in solids is assured by reference moisture determinations according to standardised procedures. According to most of these procedures, moisture is determined as the mass loss measured by weighing a sample before and after drying. However, applied drying does not extract only water but also other volatiles from the sample, and the sample after drying may contain more or less residual water depending on the state of physical or chemical binding of water in the initial sample. The effect of this ambiguity escalates in calibrations of moisture analysers with reference samples and worsens through uncontrolled water transport between a sample and its surroundings when handling the samples. The measurement uncertainty is in many cases unknown.

This JRP aims to develop unambiguous principles, methods and equipment for establishing and disseminating SI traceability to measurements of moisture in solids. This will be achieved by:

Developing unambiguous realisation methods for water mass fraction and new primary standards based on these methods.

Improving the coulometric Karl Fischer titration based realisation for water amount fraction.

Creating effective general principles of SI traceability in the field of moisture measurements.

Developing new/adapted CRMs and novel transfer standard instruments to enable dissemination of SI traceability with optimal accuracy.

Developing methods for quantifying and reducing the effect of moisture change during transporting and handling samples.

Developing a novel calibration facility with SI traceability for surface moisture meters.

Developing modelling to include local moisture variations in the uncertainty estimations, and developing uncertainty analysis tools for selected industrial applications.

Establishing a coherent and developed moisture metrology infrastructure in Europe.

The work focuses on the following material groups: pharmaceuticals, polymer/plastic, foodstuffs, feed, biomass, wood based material. However, many of the JRP outcomes will be suitable for extension to wider classes of materials and applications.

New calibration, research and expert services and new CRMs created in this JRP will be exploited by stakeholders in industry, science and metrology communities in developing new products, measurement instruments and services as well as implementing traceability for quality control. Recommendations, reports and best practice guides will help international metrology and standardisation organisations and accreditation bodies to make decisions and develop/improve documents related to moisture measurements. Best practice guides and training material will help laboratories of different kinds to develop their moisture measurement capacity. Workshops, meetings, e-Newsletters and the project website will ensure efficient exchange of information between the JRP-Consortium, collaborators and other stakeholders.

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B1.b Need for the project

Reliable moisture measurements in solids are very challenging and the actual measurement uncertainty is in many cases unknown. Among numerous unsolved problems in moisture metrology, the most fundamental one is a need to move away from method-based standardisation of procedures, towards outcome-based verification of measurement results through meaningful calibrations with traceability to the SI, disseminated in terms of mass fraction and amount fraction. At present the quality of moisture measurements in solids is assured by reference moisture determinations according to standardised procedures. The procedures are material specific and the obtained results are distorted by ambiguity of the actual measurands defined by the procedures. Industry seeks unambiguous and feasible SI traceability through calibrations and CRMs, which would improve the quality of moisture control and enable a leap forward in developing real time process control based on on-line moisture measurements.

Some 70 % of all production industries use drying of their products, for removal of water or another solvent by evaporation, as a final production step before selling or packaging solid material products. Yet direct measurements of “dryness” are under-used, due to insufficient reliability and lack of traceability in moisture measurements. Unreliable moisture measurements affect product quality and lifespan, process speed/throughput, market price by weight, re-work, and wastage. A large proportion of production processes depend on measurement or control of moisture in some form. In manufacturing this includes food, pharmaceuticals, chemicals, paper, numerous plastic and metal products, and packaging of a wide variety of items. Other sectors include agriculture (grain and other food crops), timber, civil engineering (concrete), building structures (plaster, wood, composite building components), conservation of historic artefacts, earth sciences (soil moisture and its effect on pyrgeometry), biomass for energy production, and others.

In chemical metrology, moisture is critical wherever substance purity is concerned, especially where this involves certified reference materials. Wherever any chemical or physical measurement (for example radioactivity) is referenced to dry mass of a sample, determination of moisture content directly affects results.

Even in the limited cases where air humidity in equilibrium with material is used as the main parameter describing the moisture in materials (water activity), reliable relationships between the equilibrium humidity and the moisture content (sorption isotherms) are vital for product quality control.

In various applications of process industry, in-line measurements are performed by means of microwave or NIR techniques in order to measure and control the moisture content of the products, but the final quality control of the product is most often made by mass loss on drying or titration methods. Due to method dependency, different reference methods, and lack of knowledge of the actual uncertainty, the measurements are not comparable, often leading to heavily decreased process speed/throughput and increased wastage.

Selected examples of specific needs include:

• Some 80 % of manufactured products start in the form of particulate or granular raw material. Surface and bulk moisture in powders affects flow and packing density, and determines the risk of flaws in the formation of metal, plastic and ceramic components.

• Pharmaceuticals require control of bulk and surface water content to enable press-forming of tablets, but more importantly because water affects the morphic form of active ingredients (crystalline or amorphous), affecting both bioavailability and shelf life of medicines.

• In polymer processing, excess water can lead to hydrolysis, chain scission, and foaming in extreme cases. In use, water content impairs polymer electrical insulation properties and tensile strength.

• Manufacturing of carbon-fibre composites is critically dependent on a proper moisture control in the matrix process preparation. It has been observed that moisture absorption by structural epoxy-matrix has a deleterious effect on the mechanical properties (bending strength and hardness) of the composites.

• Moisture in foodstuffs and various biomaterials is measured for reasons of quality and storage life. Reliable measurements are difficult because of unstable biochemical matrix of samples and the matrix highly depends on the source of the raw material.

• The quality of novel paper-based products such as cellulose-based active paper, as well as that of traditional paper products, is highly dependent on moisture content. The most significant paper properties affected by change in moisture level are dimensions, flatness, conductivity, strength and fold. Most of these are also important moisture dependent parameters for other wooden materials – such as package materials and finished wood products.

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• Fair trade of numerous goods by weight depends on water or moisture content. Allowable content dictates the amount and cost of processing. For example, straw biofuel measured to be outside a specified moisture range is subject to extra pricing penalties – in Denmark 1 % in straw moisture content corresponds to 1 M€ per annum.

There are more than 1300 documentary standards published by ASTM, ISO and CEN in active use in various fields of industry containing procedures related to moisture content determinations. The EA database (www.european-accreditation.org) lists 78 accredited testing laboratories in Europe that have moisture content determinations in their scope of accreditation. In addition, moisture measurement is a component of a far wider set of accredited activities.

B1.c Progress beyond the state of the art

Overview of the state of the art

At present in most moisture measurement applications, the mass Loss on Drying method (LoD) is recognised as the ultimate reference. Due to the material dependence of results obtained with the method, it has many variations described in a number of documentary standards drawn up for different materials. Confidence in these moisture measurements is based on the standardisation of measurement procedures, together with (ideally traceable) weighings, but this does not guarantee metrological traceability, because there is limited assurance on the dependence between measured mass loss and initial moisture in a sample: It is not necessarily only water that is extracted from a sample and the sample is not necessarily completely dry during weighing after drying. Alternatively, coulometric Karl Fischer titration (cKF) is in use as the reference for amount fraction measurements in some application fields. Various moisture meters and analysers of many kinds are used in laboratory and on-line applications but the calibration of them is often unsatisfactory due to the absence of appropriate reference materials, lack of calibration services and problems with handling samples. Often calibrations are not in terms of the measured quantity (mass fraction or amount fraction). Certified reference materials for moisture can provide traceability in terms of composition (fraction) but are available for only a few materials and so are often narrowly applicable. Detailed descriptions of the state of the art and how the technical work packages will deliver progress beyond it are given below:

SI moisture units and their realisation

Moisture metrology spans both physical and chemical fields. In primary moisture measurements, mass fraction or amount fraction in a measurement sample is determined by the LoD and cKF methods, respectively. Although the traceability of mass measurements to the SI base unit kilogram is fairly straightforward in the LoD method, the traceability of mass fraction is not robust because the mass of removed water during drying is not only dependent on the mass fraction but also on the degree of binding of water and the chemical matrix of the sample. The same holds when applying cKF to primary measurements of solid samples, the degree of binding of water affects the results if the water is released from the sample by heating. If the solid sample is dissolved in a suitable dry solvent, interfering compounds in the sample may significantly affect the results. Oven Karl Fisher techniques address solvent interferences, but introduce the problems of LoD methods. The uncertainty analysis methods that have been up to now applied for both LoD and cKF are not comprehensive enough for primary standards serving as the ultimate source of SI traceability in the field of moisture measurements. Published articles dealing with applying cKF to solid materials do not include rigorous estimates of measurement uncertainty. As an example of the problem with realising the moisture unit, CIPM has discussed the need for a CIPM key comparison and CMCs for grain moisture measurement among NMIs or their designates, but has found this difficult to set up, because the measurement is associated with method-dependence and the measurand is ambiguous [7].

To address this issue, the LoD and cKF methods will be investigated and new unambiguous principles of realising SI units for moisture will be developed in WP1 of this JRP. In accordance with these principles, new types of LoD primary standards will be developed comprising overall mass loss determination and measurement of removed amount of water. Uncertainty components affecting primary LoD and cKF measurements in selected materials will be investigated comprehensively in detail for the first time. As a result of this work, overall uncertainties several times better than the existing state of the art – between 0.5 and 4 per cent of value depending on material, method and range (can be significantly higher for lower ranges) [5] – will be achieved.

Dissemination of SI traceability: reference materials and sample handling

Reference materials and sampling for reference measurements are key methods in the quality control of moisture meters and analysers in industry. A few certified reference materials exist for water or moisture

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content but their application fields are narrow and their long-term stability is unreliable. A UK survey of 66 industrial and research users found existing CRMs for moisture or water are viewed as: unsuitable for instrument type (50 %); unsuitable for material type (43 %); and/or too unstable (25 %) [3]. Some commercially-available CRMs for moisture do not appear to have measurement traceability at all, and seem to be assigned unrealistically small uncertainties. It is also a concern that certification of a wide variety of matrix reference materials depends on reliable analysis of water content in the (often complex) material, which is not always available with appropriate measurement traceability, even in NMIs. Reference materials for solids with certified moisture values provided by IRMM/JRC and NIST are limited to a few food products [6, 7]. Because of the limited availability of certified reference materials, the quality of on-site moisture measurements is usually controlled by taking reference samples from process to a laboratory for LoD or KF analysis. Changes in the moisture content and inhomogeneity in the samples during transportation are not controlled or quantified. In many cases the samples are biomaterials which are not stable over time.

In WP2 of this JRP, new and/or improved certified reference materials for moisture will be developed by studying candidate materials with desirable properties, and refining certification techniques. In particular, improvements are foreseen in stability and relevance to different materials and methods. Packing/unpacking and transporting methods of reference materials and measurement samples will be studied to develop procedures ensuring better quality moisture determinations.

Dissemination of SI traceability: transfer standards

In many applications the traceability could also be disseminated using a moisture analyser as the transfer standard. However, the ambiguity of the actual measurand related to the binding of water in existing moisture meters is a limiting factor for the achievable uncertainty which is often insufficient for both dissemination of traceability and for carrying out interlaboratory comparisons at a high quality level.

A novel transfer standard based on microwave moisture detection will be developed in WP2 of this JRP. This type of instrument will detect both total moisture and the degree of binding of water. In several applications, existing microwave moisture measurement techniques have been found to be almost insensitive to density variations in the material to be measured. When combining this with the detection of water binding in a transfer standard, the uncertainty due to variations in sample material will be significantly reduced in interlaboratory comparisons and dissemination of SI traceability. To extend the range of applications, another type of system will be developed by combining microwave techniques and a stable internal reference.

Dissemination of SI traceability: surface moisture

The capability to cope with large local moisture gradients in the measured material is an essential feature of surface moisture meters. Present calibration methods, however, do not address this at all and the effect of moisture gradients are not taken into account in analysing the calibration results.

A significant improvement will be achieved in WP2 of this JRP by developing a new calibration method which will take into account the near-surface moisture gradients affecting the reading of the surface moisture meter under calibration.

Scientific tools for moisture metrology

Modelling is a powerful tool for studying moisture gradients and transport when combined with appropriate experimental validation. Moisture modelling has been widely applied to various materials and applications. However, further development is needed to obtain tools which meet the needs of foreseen developments in primary moisture realisations and dissemination of traceability in moisture. In particular, development is needed in terms of applicability to sample types and conditions relevant to the scope of this JRP, and applicability to measurement uncertainty estimations at a high quality level. For industrial measurements, appropriate uncertainty analysis tools are needed to enhance uncertainty estimations in industry as an essential part of traceability.

WP3 of this JRP is dedicated to developing modelling relevant to moisture metrology. The development will be carried out for the materials and conditions relevant to the work in the other WPs. The models will be used for estimating uncertainties due to moisture gradient related error sources and designing new calibration systems. Additionally, scientifically sound uncertainty calculation tools with appropriate user friendliness will be developed for selected industrial applications.

Metrology infrastructure for moisture

Metrology of moisture in materials is multidisciplinary. NMIs with moisture capability often address this within thermometry/humidity laboratories (because of the interaction with air humidity), or in chemistry, or partly in other areas where relevant metrological techniques are researched or used (RF/microwave/sub-millimetre electromagnetic radiation, mass, electrical, radiometry, and so on). At the international metrology level,

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moisture is in the remit of a variety of CIPM CCs and RMO technical committees. The treatment of the subject is fragmented because it spans several metrology fields and it is difficult to ensure a cross-disciplinary view. On the other hand, the moisture traceability services at NMI level are very limited, e.g. there are no CMCs on moisture in solid materials in the CMC database published by BIPM.

This JRP aims at a coherent moisture metrology infrastructure in Europe in which NMIs specialise in different subfields of moisture measurements but collaborate closely with each other. Through active cooperation with the JRP collaborators in EURAMET, COOMET, APMP, AFRIMET and SIM and participation in the work of CIPM CCTs and CCQMs, the JRP-Consortium will significantly enhance the coherence at a global level as well. In addition, the principles and practices demonstrated in the project will be implemented at all levels in the traceability chain, to promote best practice in accreditation, calibration, and testing, so that an effective metrology infrastructure for moisture reaches right down to the end users of measurements.

B1.d Overview of the scientific and technical objectives

The aim of this JRP is to enable improved dissemination of SI traceability to moisture measurements in industry throughout Europe by removing ambiguities and inconsistencies in moisture measurement and calibration techniques. This will be achieved through development of new more relevant and effective methods of realising and disseminating SI units of moisture and provision of metrology infrastructure for moisture measurements.

State of the art• LoD as the reference method:

• Actual measurand includes volatiles

• Varying binding of water

• Specific to materials

• Procedure dependent results

• LoD and cKF are not equivalent within

the unit conversion

• cKF: Improvements needed for verified

uncertainties

• Only a few appropriate CRMs available

• Traceability of the CRMs is often missing

• Transfer standard instruments are poor

due to material specificity

• Errors during handling/transport of samples

• No calibration method for surface moisture

• No tools for estimating uncertainty due

to moisture gradients or transport

• No appropriate practical methods for

estimating uncertainty in moisture

measurements

• Moisture metrology is multidisciplinary

and fragmented

• Resources of NMIs are limited

• Metrology services at NMI level are very limited

WP1: Realisation of moisture units• Unambiguous realisation of water mass fraction

• Primary standards with uncertainties better than 0.5 %

(incl. links to classical methods)

• Unambiguous principles of SI traceability

WP2: Traceability and dissemination• New CRMs with traceability and improved stability

• New transfer standards for wide range use

• Methods for quantifying and reducing the effect of

sample transport

• New calibration method for surface moisture meters

WP3: Metrological underpinning for moisture• Modelling tools for including local moisture variations in

uncertainty estimations

• Practical but metrologically sound methods for estimating

uncertainty

All WPs• Coherent European infrastructure

(specialized NMIs, globally networked,

calibration and expert service)

Robust basis

for SI

traceability

for moisture

in solids

Appropriate

methods

available for

disseminating

SI traceability

to industry

Appropriate

modelling

methods

available for

moisture

metrology

Acknowledged

NMI level

metrology

services

available for

industry

METefnet Objectives Target

| Pharmaceuticals | Polymer/plastic | Foodstuff | Feed | Biomass | Wood based materials |

Figure 1. Overview of the objectives of the METefnet JRP

More specifically, the JRP addresses the following objectives:

Realisation of moisture units (WP1):

Develop realisation methods for moisture in solids in terms of water mass fraction and amount fraction providing unambiguous traceability to SI base units.

Develop new primary standards based on the realisation methods featuring

o uncertainties better than the existing state of the art (which for NMIs is at best anywhere between 0.5 % and 4 % of the measured value depending on method and range – much worse for trace ranges).

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o a link to results obtained with the appropriate standardised (classical) LoD method.

o sample size between 25 mg and 200 g.

Establish, operate and publicise effective unambiguous principles of SI traceability, ultimately to the base units of mass or amount of substance, directly disseminated in terms of derived quantities amount fraction and mass fraction.

Dissemination of SI traceability to industrial users (WP2):

Develop new or adapted CRMs aiming to improve some or all of: stability, relevance for different measured materials, and/or for different measurement techniques. The CRMs will provide traceability to SI units as maintained by NMIs and DIs.

Develop a novel non-destructive transfer standard for reducing the effect of variations in the degree of binding of water in the measurement samples relevant to interlaboratory comparisons and for dissemination of traceability. A capability for using the transfer standard with CRMs in well controlled conditions will be developed.

Develop methods for quantifying and reducing the effect of moisture change during transport and handling of samples relevant to disseminating traceability and carrying out interlaboratory comparisons (proficiency tests).

Provide traceability to surface moisture meters by developing a novel calibration facility with SI traceability.

New scientific tools for moisture metrology (WP3):

Develop modelling relevant to moisture metrology – especially for moisture profile and transport in materials – to include local moisture variations in the uncertainty estimations and thus increase the accuracy of the monitoring capabilities of moisture sensors.

Develop uncertainty analysis tools for industrial measurements to enhance appropriate uncertainty estimations vital for obtaining traceability in on-site measurements. The analysis tools need to be appropriately simple but metrologically sound.

Metrology infrastructure (all WPs):

Establish a coherent and developed moisture metrology infrastructure in Europe – featuring NMI/DI standards and the specialisation of NMIs in different moisture fields. The work will be targeted to support the implementation of key comparisons, CMC declarations and reviews, commercial laboratory accreditations and proficiency tests, and dissemination through traceable calibrations, although not all of these will be within the project, or during its lifetime. The JRP will also deliver knowledge transfer in the form of training, workshops, publications and other information exchange with stakeholders in industry as well as research and technology organisations needing traceable moisture measurements. Cooperation will be promoted between the diverse existing committees and working groups with interests in this interdisciplinary metrology area.

Many of the JRP findings and methodologies will be suitable for extension to wider classes of materials and applications. For example, the outcomes of this project are extensible to grain moisture and thus support efforts to extend SI traceability to an area under discussion within the CCQM [8].

B2 RELEVANCE TO THE OBJECTIVES OF THE EMRP

B2.a How the JRP addresses the overall objectives of the EMRP

Integration and Efficiency

This JRP combines efforts in 10 national metrology research programmes in Europe to achieve advancement in moisture metrology never seen before and which is unreachable in fragmented activities. Furthermore, this JRP brings together groups working in physical and chemical metrology which in many countries are located in separate institutes. As the expertise relevant to moisture in materials is fragmented in Europe and within the participating countries, the moisture metrology community is weak and inefficient, without strength enough to advance the SI traceability to the required level. By bringing together these

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researchers in institutes with very different sizes and capabilities, we will achieve results with significant global impact and create unique moisture metrology services for industry.

Several institutes in countries with a small overall contribution to the EMRP have a significant role in this JRP-Consortium. One of them is BRML, which has nominated this project as the key strategic priority for Romania.

Developing metrology capacity

An integral part of this JRP is to create new metrological capabilities and services to fulfil the needs of European industry. With the foreseen results and increased expertise, the European metrology community will be able to take a leading role in the moisture field and thus enhance the competitiveness of European industry in global markets. With a strategy of distributed expertise combined with strong collaboration, the strengths of different types of metrology institutes and groups will enhance capacity building in all collaborating institutes.

Liaison with other NMIs and DIs in Europe and other regions is recognised as an important task in this project. This will enable scientific and technological input from institutes outside the JRP-Consortium and the exploitation of the results of this JRP in capacity building in other countries. In particular, countries in Europe and the near regions will be able to benefit from the outcomes through the planned training and consultation activities and the EMRP Researcher Mobility Grant Scheme.

Stimulating innovation

The fundamental work of this JRP on SI traceability will remove a barrier to progress in the reliability of moisture measurements, thus enhancing the development of moisture measurement based process control in industry. Improved accuracy in reference measurements and dissemination of traceability will give a boost to the development of improved moisture measurement instruments and materials with better moisture related properties. In particular, this JRP will create a basis for the development of innovative solutions for traceable on-line moisture measurements.

The development of measurement and sample handling methods as well as uncertainty estimation methods and tools will advance the development of commercial calibration and measurement services.

The involvement of several instrument manufacturers and service providers as collaborators (see Section G) will serve as a direct route for stimulating innovations in industry.

Involvement of outside researchers

Excellent researchers from outside the EMRP metrology community will be involved in four ways:

1. A Researcher Excellence Grant is included in this JRP to strengthen the expertise of the JRP-Consortium in modelling.

2. Stage 3 Researcher Excellence Grant positions will be advertised to address research topics specific to on-line measurements and/or for widening the scope of the work on new CRMs.

3. Researchers at NMIs outside the EMRP will be involved as collaborators and through the liaison activity tools of WP4.

4. Researchers at universities and research institutes will be involved through active interaction in relevant scientific conferences and by publishing articles in widely recognised scientific journals.

B3 POTENTIAL IMPACT THROUGH THE DEVELOPMENT, DISSEMINATION AND USE OF THE PROJECT RESULTS

B3.a Projected impact of the JRP

Direct Impact

This JRP creates direct impact for the following stakeholder groups: - the metrology community in Europe and outside - accredited calibration and testing laboratories providing services to industry - industrial laboratories assuring the quality of moisture measurements in their companies - manufacturers of moisture measuring instruments - industrial and academic groups carrying out research and development on materials - standardisation bodies

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- accreditation bodies - users of moisture meters and analysers

The research of this JRP will benefit the stakeholders in the following way

- The JRP outcomes will enable NMIs and DIs (in addition to those in the JRP-Consortium) to introduce primary standards for moisture in solids by applying the methods developed in the JRP for the realisation of moisture units and uncertainty analysis, and by carrying out comparisons against the primary standards constructed in this JRP. If a secondary standard is chosen as a national reference, the JRP-Partners will be able to disseminate the SI traceability budget to the NMI/DI and organise necessary interlaboratory comparisons for the NMI/DI. In the comparisons and dissemination of traceability, new CRMs and transfer standards, to be developed in WP2, will have a key role in achieving high quality results. NMIs and DIs will also be able to set up calibration systems for surface moisture meters on the basis of the developments and findings of WP2, and to exploit the mathematical models developed in WP3 in estimating the uncertainties due to moisture gradients and transport.

By establishing national standards on the basis of the JRP outcomes, NMIs and DIs will become able to disseminate traceability to accredited and industrial laboratories in ways not previously possible.

- As the high quality and worldwide recognition of the research findings of this JRP will be ensured by close collaboration with other NMIs and interaction with researchers in universities and other research institutes, the findings will enable regional metrology organisations and CIPM to make plans for key comparisons and CMCs relevant to moisture in solids and give guidance on moisture quantities and units and their realisation.

- Accredited and industrial laboratories will be able to improve their moisture measurements by obtaining traceability to their reference standards from the JRP-Partners through the new CRMs or transfer standards or samples of their own and by adopting the calibration and uncertainty analysis methods and tools developed in the JRP. Outcomes of the research on handling and transporting samples will able to take appropriately into account the relevant error sources and to reduce the measurement uncertainty. Best practice guides, drawn up in WP4, as well as training and expert services provided by the JRP-Partners will help the laboratories in developing their expertise and services.

Because of the developed principles of SI traceability, accredited laboratories will be able to introduce new calibration services for moisture instruments, for disseminating SI traceability to their customers in industry.

It is foreseen that for practical reasons many industrial laboratories will primarily continue providing gravimetric reference moisture measurements according to existing documentary standards. These laboratories will be able to better understand and study the effect of variations in their samples with respect to the amount of non-water volatiles and state of physical or chemical binding of water. It will become possible for them to validate their measurements by sending samples to the JRP-Partners for direct comparative analysis between documentary standard based moisture determination and SI traceable moisture measurement.

- The calibration and research facilities developed in this JRP will be exploited by moisture instrument manufacturers in terms of calibrations and tests supporting R&D activities. They will also benefit from the expertise developed in this JRP through JRP-Partners’ consultancy/expert service. Altogether, this will enable instrument manufacturers to develop new, more accurate, instruments and measurement solutions and to promote sales of them with SI traceability. The 2012 forecast market value of moisture instrument sales worldwide was about 200 million USD [9].

- Material research and development in industry and universities will benefit from the new measurement facilities developed in this JRP through measurement services provided by the JRP-Partners producing more comprehensive information on the moisture in materials. This will support innovation leading to the development of new and improved materials of all kinds.

- Standardisation bodies will get input to their work on developing and updating standards for determination of moisture in solids. In particular, data obtained on the effect of volatiles and the degree of binding of water as well as developed primary realisation methods and uncertainty analysis methods will benefit documentary standards. Just as importantly, the use of CRMs and other newly-available measurement traceability for moisture will be proposed wherever possible for inclusion in standards. The input to appropriate standardisation committees/working groups will be

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provided through the (new) participation of JRP-Partners and collaborators in the relevant committees.

- Accreditation bodies will benefit from the expertise gained in the research in the form of recognised principles of SI traceability, potential qualified technical assessors and potential organisers of proficiency tests.

- Finally, end-users, i.e. industrial users of moisture measurement instruments of various kinds, will benefit from the JRP through the possibility to obtain traceability in their instruments and measurements, leading to more reliable measurements.

End-users will also exploit the Best Practice Guides drawn up in the JRP as well as training and expert services provided by the JRP-Partners.

The benefits at the end-user level will later increase many-fold through progress initiated by this JRP in other stakeholder groups.

Long term indirect impact

Energy saving

European industry consumes some 3.5 x 109 GWh of energy per year – roughly 15 % of this in drying by

thermal or other methods. In practice, where there is any doubt about measured values of product moisture, a safety margin is often applied, resulting in over-drying and associated energy cost. Better moisture measurement can enable reduction of drying tolerances. Every 0.1 % reduction in over-drying could save around 5 x 10

5 GWh per year across Europe (equivalent to several power stations). Reductions of several

times this are realistically possible. In a specific case: pulp and paper production in Europe amounts to about 55 000 tonnes per annum, with more than 60 GWh of energy spent per year. A 0.1 % improvement in control of moisture conditioning processes could save up to 8 MWh per annum. Across all sectors, more reliable moisture processing can also reduce failures in product quality, so that reductions in re-work can give further energy savings.

Environmental

Reduced energy consumption arising from fine-tuning of moisture-critical processes reduces carbon emissions. Every 0.1 % cut in industrial energy use prevents around 2 x 10

5 tonnes of CO2 emissions per

annum across Europe. The impact of better moisture measurements on growing efficient uptake of low-carbon biofuels can further reduce emissions, as both the calorific value and critical handling properties of biofuels depend on water content. Across a wide range of production processes, reduced raw-material wastage, and also reduced waste disposal to landfill, will also have environmental benefits.

Financial

Drying alone is estimated to cost European industry some 50 000 M€ per year (energy cost). Every 0.1 % improvement in drying efficiency due to better measurement could save around 50 M€; Europe-wide realistic savings could be several times this. As an example, across Denmark the total cost of 0.5 % over-drying is estimated to be 4.2 M€ annually in energy alone. Improved productivity of existing industrial processing plants can also bring results: in a single large milk spray-drying plant, 0.1 % in moisture content is worth 0.5 M€/year in increased throughput alone.

Product quality, fair trade, health, consumer protection and social benefits

Improved metrology for moisture will impact a vast range of areas, from trade in goods by weight, to quality of medicines and foodstuffs, to preservation of cultural heritage, and numerous others. Moisture driven mould growth in buildings is a serious health risk in many European countries. Improved moisture metrology and modelling will contribute to efforts to reduce this risk through the development of methods for preventing and monitoring moisture in building structures.

B3.b Projected JRP impact on EC Directives, and other relevant standards

Hundreds of EN and ISO standards documents address moisture measurement. Around 100 of these standards have moisture in the title and have a main focus on moisture measurement or calibration. Several hundred more standards incorporate a moisture measurement or specification as a part of the detail. Because they are such a wide and dominant influence on moisture measurement practices, published standards are an area of concern in the moisture field. As they specify reproducible moisture measurement processes, adherence to a standard can serve as a token of quality assurance for a measurement that would

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be better assured through traceable calibration in terms of the measured quantity. This is not a reason to deprecate these standards, but to underpin them with best measurement practice and SI traceability.

While many published standards embody moisture measurement practices that are fit-for-purpose, others fall short of best practice. There is scope to propose the incorporation of best practices in a variety of aspects: measurement traceability for moisture, correct estimation and expression of uncertainty (and allowance for this in tolerance pass-fail criteria), and other input.

The JRP-Partners already participate in a number of relevant standard committees (see details in Section C4.a). However, the work in WP4 goes far beyond this. A campaign of engagement with standard committees will be undertaken, both to influence moisture-related standards as they are reviewed and to spread awareness of the JRP among a target audience of standards-makers in a wide variety of moisture-related sectors. This is expected to impact upon standardisation in ISO categories of Construction materials and building, Wood technology, Manufacturing engineering, Food technology, Rubber and plastic industries, Chemical technology, and selected others.

B4 THE QUALITY AND EFFICIENCY OF THE IMPLEMENTATION AND MANAGEMENT

B4.a Overview of the JRP-Consortium and JRP management

This JRP-Consortium brings together the main European NMIs active in the field of moisture measurements. The expertise of the laboratories and scientists involved covers both physical and chemical metrology, which is essential to achieve success in this multidisciplinary work. In particular, the JRP-Consortium has strong experience in gravimetric methods (MIKES, BRML, CMI, DTI, NPL, TUBITAK), Karl Fischer titration (UT, BRML, CMI), water vapour detection (MIKES, CETIAT, DTI, INRIM, NPL, UL, TUBITAK), humidity and temperature control (MIKES, CETIAT, DTI, INRIM, NPL, UL, TUBITAK), uncertainty analysis (all JRP-Partners), modelling (CMI, DTI, INRIM, REG(UNICLAM)) and development of metrological instruments (MIKES, CETIAT, DTI, INRIM, NPL, UL, TUBITAK) and services (all JRP-Partners). The JRP-Partners have close collaboration with industrial stakeholders and are deeply involved with metrology cooperation at a European and global level.

Without multinational effort, the foreseen leap forward in moisture metrology is not possible. Contributions of several NMIs are needed to achieve a critical coverage in materials and ranges. All the JRP-Partners will contribute to the main outcomes. The work is balanced according to national industrial priorities and research strengths, resulting in optimal distribution of work but European wide impact. Through the strong links of the JRP-Partners to metrology regions outside Europe the outcomes will be exploited worldwide.

Although the work is mainly distributed with respect to material types and measurement methods, some duplication is essential to 1) verify the general validity of the developed realisation methods and principles of SI traceability, and 2) identify potential sources of systematic errors in the primary standards to be developed.

The JRP will be managed through 1) regular review of the deliverables and the progress in WPs at task level by WP leaders and the JRP-Coordinator, 2) internet meetings of the Project Management Board (consisting of WP leaders and the JRP-Coordinator) every six months, and 3) annual General Project Meetings attended by all JRP-Participants. The JRP-Coordinator is well experienced in managing international multipartner projects and he is a worldwide recognised expert in the field of humidity and moisture metrology, with a longstanding leadership role in EURAMET TC-T/SC Humidity and its work.

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Section C: Detailed Project Plans By Workpackage

The technical/scientific work aiming at unambiguous and consistent moisture measurement and calibrations through SI traceability is divided into three technical workpackages as illustrated in the following diagram. It also shows how the workpackages are related to each other

WP1: Realisation of moisture units• New approach to SI unit realisations

• Experimental validation of the approach

• New primary standards for water mass fraction

• Improved primary standards for water amount fraction

• Principles of SI traceability

• Links to classical methods

WP2: Traceability and dissemination• New CRMs

• New transfer standards

• Methods for quantifying the effect of sample transport

• Calibration method for surface moisture meters

WP3: Metrological underpinning for moisture• Experimentally validated numerical simulation models

• Model uncertainty budgets

WP4: Creating Impact• Knowledge transfer

• scientific and technical papers

• reports

• liaison with stakeholders

• conference presentations

• best practice guides

• Training

• training material

• workshops

• Metrology infrastructure

• Exploitation

• calibration and expert services

• exploitation plan for CRMs

WP5: Management and Coordination

Instrumentation for

validation and

experimental researchMethods for

intercomparisons

Instrumentation for

experimental validation

of simulation models

Numerical modelling

for instrument

development


WP1: Realisation of moisture units• New approach to SI unit realisations

• Experimental validation of the approach

• New primary standards for water mass fraction

• Improved primary standards for water amount fraction

• Principles of SI traceability

• Links to classical methods

WP2: Traceability and dissemination• New CRMs

• New transfer standards

• Methods for quantifying the effect of sample transport

• Calibration method for surface moisture meters

WP3: Metrological underpinning for moisture• Experimentally validated numerical simulation models

• Model uncertainty budgets

WP4: Creating Impact• Knowledge transfer

• scientific and technical papers

• reports

• liaison with stakeholders

• conference presentations

• best practice guides

• Training

• training material

• workshops

• Metrology infrastructure

• Exploitation

• calibration and expert services

• exploitation plan for CRMs

WP5: Management and Coordination

Instrumentation for

validation and

experimental researchMethods for

intercomparisons

Instrumentation for

experimental validation

of simulation models

Numerical modelling

for instrument

development


Figure 2. Overview of the METefnet JRP

C1 WP1: Realisation of moisture units

(MIKES, BRML, CETIAT, DTI, NPL, TUBITAK, UT)

Start month: Jun 13, End month: Mar 16

Aim

The aim of this workpackage is to create a robust basis for SI traceability in measurements of moisture in solids. This will be achieved by 1) developing unambiguous realisation methods for mass fraction (Task 1.1), 2) improving the realisation method for amount fraction (Task 1.2) and 3) establishing effective unambiguous principles of SI traceability in moisture measurements (Task 1.3). Links to existing reference methods will be retained by determining classical moisture values in parallel with the SI traceable results, which is vital for adopting the new approach widely in various fields of industry.

Background

There is a global need to move away from method-based standardisation of procedures, towards outcome-based verification of measurement results through meaningful calibrations with traceability to the SI, disseminated in terms of mass fraction and amount fraction. To enable this, unambiguous but effective principles of SI traceability for moisture measurements must be established.

In most moisture measurement applications, the Loss on Drying method (LoD) is recognised as the ultimate reference. There are many standardised variations of the method in use for different materials and applications. When drying a solid material sample, the measured mass loss does not depend only on the water content but also on the degree of binding of water and the content of volatile components in the sample. Therefore, the actual measurand in LoD measurements may significantly differ from the water mass fraction that is the relevant SI quantity. Significant improvements must be introduced to LoD based measurement standards to remove this ambiguity in the primary moisture unit realisation. Furthermore,

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uncertainty analysis methods must be developed for including the variations in water binding and volatile contents in a sound way in the uncertainty budgets for the primary realisations.

Alternatively, Karl Fischer titration methods are in use in the moisture measurement field as the reference for water amount fraction measurements in some application fields. These methods are primary because no reference in terms of moisture units is needed to obtain the water amount fraction value. Because the coulometric Karl Fischer titration method (cKF) is more accurate than the volumetric one, it is taken as the primary standard method for moisture. However, there is a need to investigate and improve the method for moisture unit realisation in solid samples. In particular, the effect of completeness of water transfer and possible transfer of interferents in the measurement cell need to be studied. The research on volatiles and water binding related to sample heating is also relevant to cKF when the sample material is insoluble to appropriate solvents.

Objectives and research methodology

The objectives of this WP and the means to obtain them are summarised in the figure below:

Robust basis

for SI

traceability

for moisture

in solids

Unambiguous realisation

of mass fraction based on

combining LoD with

complementary water

detection

Improved cKF realisation

method for amount fraction

Unambiguous

principles of SI

traceability in

moisture

Two primary

standardsStudy of LoD with water

detection:

1) electrolytic

2) chilled mirror

3) capacitive

+ cold trap

4) KF titration (+TGA)

Comparison with

classical LoD and

to each other

Experimental

methods for

uncertainty

analysis

Studies on two cKF

systems equipped with

diaphragm cell

Improved accuracy

through optimized

parameters

Improved

uncertainty

analysis

Task 1.1Task 1.1

Task 1.2Task 1.2

Task 1.3Task 1.3


Figure 3. Overview of the objectives and research methodology of WP1

C1.a Description of Work

Task 1.1: Development of gravimetric realisation methods (MIKES, BRML, DTI, NPL, TUBITAK)

(Start Jun 13, End Mar 16)

The aim of this task is to develop a general approach for the gravimetric realisation of the moisture unit of mass fraction, to test the applicability and validity of the approach, to develop primary standards based on the approach and to estimate the uncertainty of the realisation in a comprehensive way.

The approach for the gravimetric realisation will be based on combining the LoD method with a complementary water loss detection system. Being the most vital property for the realisation of a SI unit, the uniqueness of the approach will be studied extensively by introducing several complementary water loss detection methods and using them with the LoD method in selected material groups. A few of the applied methods will be developed into primary standards serving customers after the completion of the project as primary sources of traceability for moisture. As a comprehensive uncertainty analysis is vital for primary realisations, extensive research is needed to develop appropriate methods to quantify the various uncertainty components relevant to the realisation of water mass fraction. Issues to be addressed are: drying methods, determination of drying endpoint (including a threshold for release of water in different states of binding) water regain, and other spurious mass losses.

Many of the complementary water loss detection methods to be explored use gas phase detection of the water driven off during drying. This uniquely draws on established expertise of the JRP-Partners specialising in humidity metrology.

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Description of activities:

Literature review of recent developments in LoD techniques: NPL and BRML will initially review recent literature on LoD methods, especially the large number and variety of documented standard methods (EN/ISO/national documents) – both recommendations and mandatory regulations. Any significant findings will be reported to the JRP-Participants, especially those working on this task. In particular this may highlight additional areas of focus for Task 1.1 or others. (NPL, BRML) (D1.1.1)

Applying electrolytic water vapour measurement as the complementary water loss detection and developing a primary standard for small size material samples: NPL will upgrade a commercial evolved vapour analyser (comprising oven drying and electrolytic water vapour detection, together with weighing) to a primary standard by establishing traceability to weighing, thermal treatment and water detection and by studying the dependence of relative mass loss and water release on temperature thermal treatment parameters, with interpretation of state of binding and the effect of volatile components for selected materials relevant to pharmaceutical and plastics manufacture, and foodstuffs (at least 8 samples). The sample size is 25 mg to 2 g. The system can measure a full range of water contents, limited only by the uncertainties where samples contain either minimal water, or almost all water. The uncertainty target will be to improve on the current state of the art for oven Karl Fischer methods (around 4 % of measured value in most measurement ranges). The study will include evaluations of drying end points, water regain, and supporting measurements of other released volatiles using quadrupole mass spectrometry. NPL will carry out a comprehensive uncertainty analysis for the standard system and a comparison between the developed realisation method and the relevant standardised LoD method. A paper will be written on the primary standard validation. (NPL) (D1.1.2, D1.1.3, D1.1.7)

Applying chilled mirror based water vapour measurement as the complementary water loss detection and developing a primary standard for medium size samples: DTI will design and construct a primary standard comprising an LoD system (oven drying and weighing) and a chilled mirror based water vapour detection system. A novel sample containment system will be constructed for contamination free in-situ sample handling, with a capacity for samples up to a mass of 200 g and volume of 200 cm

3. The target moisture content range for the

primary standard is from 10 g/kg to 950 g/kg. The target relative uncertainty for LoD measurements is 0.5 % or better and 2 % for water vapour detection. The experiments will be carried out with powder, granular and bulk material samples relevant to foodstuffs, feed and biomass (at least three samples of each). DTI will carry out a comprehensive uncertainty analysis for the standard system and a comparison between the developed realisation method and relevant standardised LoD method. A paper will be written on the primary standard validation. (DTI) (D1.1.4, D1.1.5, D1.1.7)

Applying a capacitive water vapour detection combined with a water trap as the complementary water loss detection and developing a novel research system for various particle and sample sizes: MIKES will develop a novel research system in which the mass loss and water evaporation rate from a solid sample exposed to different heating cycles is monitored and determined by means of 1) weighing the sample in a measurement chamber, 2) capacitive humidity detection of gas passing through the chamber, and 3) weighing the water trapped from the gas flow. The sample size is 5 g to 400 g, and the target relative uncertainty in the measurement range between 50 g/kg to 600 g/kg is 2 %. MIKES will apply the system to investigate the correlations between the determined mass loss of the sample, evaporating water, evaporating other chemical compounds, degree of binding of water and different heating cycles in biomass and wooden material samples (at least three samples of each). In addition, MIKES will study the effects of different particle sizes (5 mm – 100 mm) in the sample and carry out a comprehensive uncertainty analysis for the research system and a comparison between the developed realisation method and the relevant standardised LoD method (ASTM E1868-10, EN 14774-1). The equipment will also be used in WP2 (Task 2.2). A paper will be written on the new system. (MIKES) (D1.1.6, D1.1.7)

Applying Karl Fischer titration and TGA as the complementary water loss determination: BRML will contribute to the research on the unambiguous realisation of water mass fraction by investigating moisture determinations in paper samples using its IR LoD analyser and coulometric KF equipment. The number of samples with both techniques is 5 different samples with 10 determinations each. BRML will carry out a comprehensive uncertainty analysis for the measurements and a comparison between the developed realisation method and the relevant standardised LoD method.

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TUBITAK will study the application of the gravimetric moisture unit realisation approach in plastic and paper materials in sheet form, including 20 paper sheet samples with different weights ranging from 75 g/m

2 to 420 g/m

2 and from 16 g/m

2 to 23 g/m

2, and 5 plastic/polymer samples. LoD

moisture measurements will be supported by TGA to make a distinction in analyte between water and other volatiles. TUBITAK will also compare the moisture measurements using the LoD method and coulometric Karl Fischer titration method for the same materials. Different drying temperatures will be investigated to obtain information on the degree of binding of water in the samples. The temperature range applied will be from room temperature to 500 °C for TGA, room temperature to 200 °C for LoD measurements, and from room temperature to 300 °C for Karl-Fischer analysis. TUBITAK will carry out a comprehensive uncertainty analysis for the measurements and a comparison between the developed realisation method and the relevant standardised LoD method. (BRML, TUBITAK) (D1.1.7)

Estimation of uncertainty components specific to the gravimetric realisation methods On the basis of experiments in Task 1.1, MIKES, DTI, BRML, NPL and TUBITAK will analyse uncertainty components specific to the gravimetric realisation methods of moisture unit and develop a metrologically sound way to include the effect of water binding and volatiles in the relevant uncertainty estimations. A paper will be written on the uncertainty estimation. (TUBITAK, BRML, DTI, MIKES, NPL) (D1.1.8)

Major facilities to be used: Evolved-vapour analyser, quadrupole mass spectrometer (NPL), cKF titrator, IR LoD analyser (BRML), cKF titrator, TGA (TUBITAK)

This task is dependent on input from the following deliverables: D3.1.3, D3.1.5.

This task leads to deliverables: D1.1.1 to D1.1.8.

The deliverables of this task are required for tasks: 1.3, 2.1, 2.2, 2.4, 3.3.

Task 1.2: Improved Karl Fischer titration realisation methods (UT, BRML)

(Start Jun 13, End Jul 15)

The aim of this task is to carry out an in-depth metrological study of the coulometric Karl Fischer titration (cKF) method and to propose improvements for reducing its uncertainty. The expected relative k = 2 expanded uncertainty is 2-3 times below the current state of the art, 0.5 % – 4 % (may be significantly higher for low water contents). The wide range of this estimate is caused by 1) different uncertainties in the case of different materials, and 2) very limited uncertainty information (often just repeatability of reproducibility information instead of rigorous uncertainty estimates) available in most literature sources. The reduction of uncertainty will be achieved by optimising the parameters of the KF titrator itself (stirring speed, background correction, endpoint determination, etc.) as well as the sample oven (sample size, sampling temperature, carrier gas flow rate, etc.).


UT will carry out a literature survey of the uncertainty sources of coulometric KF titration and their estimated contributions. Particular attention will be paid to moisture determination in solid materials (as opposed to liquids), such as paper and polymers (PE, PP, PS, ABS, PVC, PA). This information together with the earlier experience of the JRP-Partners will form the basis for 1) the improvements to the coulometric KF method and 2) more accurately defining the current state of the art of the uncertainty achievable for moisture determination in materials with cKF. (UT) (D1.2.1)

UT and BRML will set up the initial coulometric KF method in their laboratories. It will use a cell with a diaphragm as this cell leads to lower uncertainty. The method will be validated at both laboratories and an uncertainty budget will be compiled. Distinction will be made between the uncertainty sources of the KF titration as such (instrument stability, interferences etc.) and the uncertainty sources due to transferring the water from the sample to the titration medium. UT will focus on the uncertainty sources related to the coulometry itself. BRML will focus on the uncertainty sources related to the interaction between the sample and its environment during the analysis. The resulting information will be exchanged and both labs will apply it to their methods and will compile the uncertainty budgets of their respective methods. (UT, BRML) (D1.2.2, D1.2.3)

Based on the information from the uncertainty budget the complete method (including sample handling) will be modified in order to reduce the uncertainties of the largest uncertainty contributors as far as practical to arrive at the final method. Again, UT will focus on modifications of the coulometric KF titration itself and BRML will focus on the interactions between the sample and its

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environment. Eventually the optimal parameters will be found, giving rise to a validated method, and the final uncertainty budget will be compiled. The method will be set up at the laboratories of UT and BRML. (BRML, UT) (D1.2.4, D1.2.5)

Major facilities to be used: Two cKF titrators (UT), cKF titrator (BRML)

This task is dependent on input from the following deliverables: none.


The deliverables of this task are required for tasks: 1.3, 2.1, 2.2, 3.3.

Task 1.3: Principles of SI traceability (MIKES, DTI, CETIAT, NPL, UT, TUBITAK, BRML)

(Start Oct 13, End Mar 16)

The aim of this task is to establish effective unambiguous principles of SI traceability in moisture measurements. Task 1.1 and Task 1.2 outcomes will be analysed further and interlaboratory comparisons will be arranged. The comparison results will be used for probing the general validity of the findings and for informing the design of future comparisons at more formal levels (such as CIPM or RMO key comparisons). Recommendations on unambiguous principles of SI traceability for the moisture metrology field will be formulated and published.


Review of terms and definitions used in moisture measurements NPL will review the state of the art of definitions of quantities, units, symbols and terminology, both within the SI and in wider usage, for both water content and moisture content. This will draw together various available information, and will identify areas for action in support of coherent usage across metrology infrastructure in Europe and more widely. The consultation will include interested bodies such as CCQM, CCT WG6, and various JRP-Partners, collaborators and stakeholders as appropriate. (NPL) (D1.3.1)

Interlaboratory comparisons 1) UT, BRML and TUBITAK will carry out a comparison between the cKF moisture determinations (at UT and BRML) and the LoD determinations (at TUBITAK). Polymer samples with two different moisture content levels will be selected for the comparison (one sample provided by BRML and one by UT). (UT, BRML, TUBITAK) (D1.3.2) 2) NPL, DTI, BRML, CETIAT, MIKES and TUBITAK will carry out a comparison in which foodstuff and biomass relevant samples (two to five samples) with two different moisture content levels will be measured using the methods of Task 1.1 and the transfer standard developed by CETIAT in WP2. (MIKES, BRML, CETIAT, DTI, NPL, TUBITAK) (D1.3.3) 3) NPL, DTI, UT, TUBITAK and BRML will carry out an intercomparison of the developed primary standards using the new CRM developed in WP2. (NPL, DTI, UT, TUBITAK, BRML) (D1.3.4)

Recommendation on the principles of SI traceability in moisture measurements Based on the review of terms and definitions and on the interlaboratory comparisons NPL, MIKES, CETIAT and TUBITAK will prepare a recommendation on the definitions of quantities, units, symbols and terminology for moisture content in the SI. NPL, MIKES, DTI, CETIAT, UT, BRML and TUBITAK will prepare a recommendation on the realisation of moisture units in the SI. The recommendations will be published. (MIKES, DTI, CETIAT, NPL, UT, BRML, TUBITAK) (D1.3.5, D1.3.6)

Major facilities to be used: Facilities developed in Tasks 1.1 and 1.2. The facilities will be located in the laboratories of the corresponding JRP-Partners.

This task is dependent on input from the following deliverables: D1.1.2, D1.1.4, D1.1.6, D1.2.5, D2.1.3, D2.2.5, D2.3.4.


The deliverables of this task are required for tasks: none.

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C1.b Labour Resources for WP1

1- M

IKE

S

2- B

RM

L

3- C

ETIA

T4-

CM

I

5- D

TI

6- IN

RIM

7- N

PL

8- T

UBIT

AK

9- U

L

10- U

T

11- R

EG

(UN

ICLA

M)

TO

TA

L

WP1 14.0 18.0 2.5 13.0 14.5 7.0 28.5 97.5

C1.c Summary of Deliverables for WP1

Deliverable number

Deliverable description Lead Participant

Other Participants

Deliverable type

Delivery date

1.1.1 Summary report on key findings of literature review

NPL BRML Report Nov 13

1.1.2 LoD primary standard for moisture with sample size smaller than 2 g

NPL Device May 14

1.1.3 Peer-reviewed journal or conference paper on validating NPL’s primary standard for moisture submitted

NPL Publication Nov 14

1.1.4 LoD primary standard for moisture with sample size up to 200 g

DTI Device May 14

1.1.5 Peer-reviewed journal or conference paper on validating DTI’s primary standard for moisture submitted

DTI Publication Nov 14

1.1.6 Peer reviewed journal or conference paper publishing the MIKES research system submitted

MIKES Publication Nov 14

1.1.7 Comparison data between the SI traceable moisture realisations and relevant standardised moisture determinations for selected materials in pharmaceuticals, foodstuff, feed, biomass, wood and paper

MIKES BRML, DTI, NPL, TUBITAK

Data set May 15

1.1.8 Peer-reviewed journal or conference paper on uncertainty estimation tools for gravimetric SI moisture unit realisation submitted

TUBITAK BRML, DTI, MIKES, NPL

Publication Mar 16

1.2.1 Literature survey of the factors determining the uncertainty of cKF method and their contributions

UT Report Sep 13

1.2.2 Coulometric KF measurement setups and the initial method set up at JRP-Partners' labs

UT BRML Device Mar 14

1.2.3 Report on the interaction between sample and its environment during the cKF analysis and a validated procedure to minimise the corresponding uncertainty

BRML UT Report Sep 14

1.2.4 Final cKF method including the sample handling part is available and validated

UT BRML Procedure Jan 15

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1.2.5 Validation report and uncertainty budget available for the coulometric KF method

UT BRML Report Jul 15

1.3.1 Report on the review of terms and definitions in moisture measurements

NPL Report May 15

1.3.2 Report on the comparison of the cKF results with LoD method for polymer samples

UT BRML, TUBITAK

Report Nov 15

1.3.3 Report on the comparison with foodstuff and biomass relevant samples with two different moisture content levels measured using the LoD methods.

MIKES BRML, CETIAT, DTI, NPL, TUBITAK

Report Jan 16

1.3.4 Report on the comparison of the developed primary standards using new CRMs developed in WP2.

NPL DTI, UT, TUBITAK, BRML

Report Feb 16

1.3.5 Draft document recommending terms, definitions, realisations and principles of SI traceability for moisture measurements

MIKES DTI, CETIAT, NPL, UT, BRML, TUBITAK

Discussion draft

Jan 14

1.3.6 Paper on comparisons and traceability for moisture measurements submitted to a peer-reviewed journal

MIKES DTI, CETIAT, NPL, UT, BRML, TUBITAK

Publication Mar 16

C2 WP2: Traceability and dissemination

(CETIAT, BRML, CMI, INRIM, MIKES, NPL, UL, TUBITAK, UT)


Aim

The aim of this workpackage is to develop improved methods for disseminating traceability from primary standards to industrial moisture measurements. Development of new CRMs and transfer standards with traceability to the SI plays a key role in reaching the aim (Tasks 2.1 and 2.3, respectively). To underpin traceability in applications where sampling from an industrial process is the only feasible approach for disseminating traceability, methods for quantifying and reducing the measurement errors and uncertainty due to moisture changes in samples will be developed in Task 2.2. A new, comprehensive method and instruments will be developed in Task 2.4 for disseminating traceability to surface moisture meters.

Background

Without proper means to disseminate SI traceability, development of primary moisture standards (WP1) would be mostly wasted because industry could not exploit the achieved advancements. The traceability is usually disseminated using CRMs, transfer standards or reference samples, e.g. taken from a process. All of these are mostly inadequate at present:

Few certified and standard reference materials are available for moisture. Many are material-specific, and considered to have limited wider applicability. Water is often an important but uncertified component of CRMs certified for other aspects of composition. Where water-specific CRMs exist, frequently the certified water values have been assigned by consensus, without rigorous SI traceability and GUM-compliant uncertainty evaluation. There is a strong need for a wider variety of moisture CRMs with traceability to the SI, improved metrological properties and recognised certification. These are essential in providing traceable realisation of moisture fraction, to reduce dependence of users on method-based implementation of methods, for which traceability to mass alone is not enough to assure correct and traceable measurement results.

In disseminating traceability or carrying out interlaboratory comparisons, use of a transfer standard instrument instead of reference materials is especially profitable in applications of biomaterials with poor stability even in the short term. When using a moisture measuring instrument as a transfer

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standard, major characteristics defining the achievable uncertainty are portability, stability, and insensitivity to variations in chemical matrix in samples, i.e. if the characteristics of the instruments tend to drift in the long term and/or variations in the content of other volatiles or binding of water significantly affects the results, the probability of poor results in a comparison or calibration performed with the instrument is very high. Although there are fairly stable and water-specific moisture meters commercially available, they don’t indicate whether “free” or “bound” water is measured, which is essential when establishing traceability to the primary moisture standards.

Because of the large variety of materials with different properties affecting moisture measurements, reference measurements for samples taken directly from process will also have an important role in the future. In many cases, however, the reference measurements are distorted by moisture exchange between the sample and its surroundings during handling and transportation of the samples. Consequently, measurement errors are often significantly larger than the uncertainty of the reference measurement. Developments are needed to reduce the errors and estimate the total uncertainty of the reference moisture value relevant to the customer.

Several invasive or non-invasive moisture sensors (such as resistive, capacitive, microwave and NIR) are used for measuring surface moisture of materials at a declared depth. The raw signal of the sensors responds to the aggregate moisture level of a certain layer of the material which differs from the bulk moisture level due to significant moisture gradients close to the surface. Therefore, usage of reference samples with SI traceability does not ensure adequate reliability in the calibrations of surface moisture meters. The effect of moisture gradients need to be studied and included in the analysis of results as a part of the calibration procedure.


As shown in figure below, this WP addresses four types of methods to disseminate SI traceability relevant to moisture measurements in solids. For each type, new methods and artefacts will be developed to establish or improve the dissemination of traceability.

Moisture analyzers in

industry

Industrial in-line

moisture measurements

Surface moisture meters

in industry

Primary standards

for moisture in

solid materials

CRMs for wide

range of materials

Transfer standard

instruments

e.g. for biomaterials

instable in long term

Reference

samples

from

process

Calibration

system- not available yet

New CRMs- SI traceability

- Improved moisture

characteristics

New instruments- two approaches for

wide coverage in

applications

Methods for quantifying

and reducing errors in

handling and transporting

samples

Novel calibration

systems incl.

determination of controlled

moisture gradients

Dissemination methodDissemination method Development in this JRP Development in this JRP

Task 2.1Task 2.1

Task 2.3Task 2.3

Task 2.2Task 2.2

Task 2.4Task 2.4 .


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Task 2.1: New CRMs (NPL, BRML, UT)

(Start Jun 13, End Sep 15)

The aim of this task is to develop new or adapted CRMs with SI traceability aiming to improve some or all of the following: stability, relevance for different measured materials and/or for different measurement techniques. This may involve the use of novel reference materials as well as refinement of the certification technique and reporting.

Candidate materials will be considered based on desirable properties such as stability, ease of use, availability in bulk and in purity, compatibility with multiple methods, distinct water (with or without other volatiles) and in a distinct state of binding. In some cases materials will be considered which are already certified for other aspects of composition, or are analogues for materials of special user interest, or have other potential advantages. Example “simple” materials include hydrates of chemical salts (range of water content spanning several to tens of per cent). Example “application-identical” materials would include polymers, pharmaceutical fillers or diluents (such as lactose), and material types already used in CRMs but not yet certified for water (wide variety of reference substances, usually with only trace amounts of water).

The study will look at techniques of use with rigorous measurement traceability and realistic estimates of uncertainty. The work will employ combined classical and water-specific LoD methods, and mass-spectrometry (NPL) and the cKF method (BRML, UT) to distinguish water from other volatiles. This will include an assessment of uncertainty due to drying end point and ambient water regain. Using the primary measurement validated in Task 1.1, estimated absolute values of water mass/amount fractions and uncertainties will be assigned to one or more CRM. Example certification will demonstrate SI traceability with suitable reporting of measurement uncertainty.

Collaboration in this task will be provided by LGC (UK), who will advise on candidate materials, and Karl-Fischer techniques and uncertainties. Two UK Collaborators with pharmaceutical interests have also offered input (UCL and Intertek).


BRML, NPL and UT will draw up a list of candidate materials to study, specifically with relevance to water content while considering the presence of other volatiles. (NPL, BRML, UT) (D2.1.1)

BRML, NPL and UT will study the candidate materials and carry out an uncertainty analysis on one or more for certification as a CRM. (NPL, BRML, UT) (D2.1.2)

NPL, BRML and UT will make at least one CRM available to JRP-Partners and Collaborators for trial measurements. Exploitation of the developed CRM(s) will be addressed in WP4. (NPL, BRML, UT) (D2.1.3)

Major facilities to be used: Coulometer Karl-Fischer titrators with diaphragm cells (BRML, UT); LoD facilities: Mettler Toledo IR moisture analyser (BRML) water-specific evolved-vapour analyser Sartorius WDS 400, and TA Instruments Q500 TGA, quadrupole mass spectrometer (NPL)

This task is dependent on input from the following deliverables: D1.1.2, D1.1.3, D1.2.4.


The deliverables of this task are required for tasks: 1.3, 3.2.

Task 2.2: Improved methods for handling and transporting samples (MIKES, BRML, CMI, INRIM, TUBITAK)

(Start Jun 13, End Sep 15)

The aim of this task is to quantify and reduce the measurement errors and uncertainty due to moisture changes in samples during transportation. This is achieved by 1) introducing continuous ambient monitoring for the sample transportation, 2) studying experimentally the effects of various parameters on samples relevant to transportation, 3) developing analysis methods for estimating the uncertainty, 4) exploring possibilities to introduce a correction factor for minimising the error due to the moisture changes and 5) writing a good practice guide for sample transportation with appropriate links to existing guidance documents for sampling.

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The work is focused on temporal and spatial moisture variations during packing, transportation, storage, unpacking and preparing for analysis. The effects of environmental conditions (ambient temperature and humidity), exposition time, packaging materials and package closing techniques will be studied.


Review of current practices BRML will review standardised and other procedures relevant to the transportation of samples and CRMs. (BRML) (D2.2.1)

Transportation methods for processed wood and biomass samples MIKES will use NIR, IR and/or NMR instruments and the research facility developed in WP1 to study the effects of varying conditions and packaging methods on processed wood and biomass samples (plywood and woodchips, both with at least three moisture content levels) while packing, transporting, unpacking and crushing them for LoD analysis. From the results, MIKES will analyse the corresponding effect on the uncertainty when following generally used procedures. A simplified RH/T logger based method will be developed for monitoring the conditions in sample containers and for determining the effect on the final moisture determination. The NIR and/or NMR instrument(s) will be loaned by a collaborator (Metso Automation). A paper will be written on RH/T logger based method. (MIKES) (D2.2.2, D2.2.3)

Effect of sample preparation and transportation conditions on timber samples CMI will investigate the influence of different sample preparation and handling techniques on the stability of timber samples by gravimetric method and electrical moisture meters. In addition, the effect of ambient conditions on the structure and parameters of wood affecting electrical moisture measurements and overall sample quality will be investigated. A paper will be written. (CMI) (D2.2.3)

Development of multipurpose sample holders for the microwave transfer standard INRIM will design and evaluate at least three multipurpose sample holders: for transferring samples to and from the laboratory and the test site; for maintaining a stable environment for a moist sample; and for actively conditioning a sample by proper setting of its boundary conditions. The holders will be designed to be assembled as a part of the microwave moisture meter transfer standard developed in Task 2.3 where dielectric resonator, conductive resonator or waveguide measurement methods will be implemented. (INRIM) (D2.2.4)

Study on transportation methods for highly hygroscopic samples In this study special attention will be paid to packing, unpacking and sealing the samples for transportation. BRML will study 3 different samples of food and 3 different samples of pharmaceutical powders selected for their moisture instability using cKF and NIR analysers. TUBITAK will study paper samples with LoD and NIR analysers. 20 paper sheet samples with different weights ranging from 75 g/m

2 to 420 g/m

2 and from 16 g/m

2 to 23 g/m

2 will be studied.

BRML and TUBITAK will compare the findings with procedures in general use and analyse the corresponding uncertainty limits. A paper will be written. (BRML, TUBITAK) (D2.2.5)

Potentiality of applying a correction factor to reduce the effect of transportation Using the results obtained in this task, MIKES and CMI will analyse whether a correction factor related to ambient conditions during transportation can be determined for wooden samples and if it improves the reliability of the reference moisture measurement. (MIKES, CMI) (D2.2.6)

Good practice guide for estimating the uncertainty due to sample handling and transportation MIKES, CMI, BRML and TUBITAK will writing a good practice guide for sample handling and transportation with appropriate links to existing guidance documents for sampling. (CMI, BRML, MIKES, TUBITAK) (D2.2.7)

Major facilities to be used: Coulometer Karl-Fischer titrator (BRML); Able&E-Jasco Spectrophotometer (BRML); the novel LoD research system (MIKES), LoD and microwave analysers (TUBITAK)

This task is dependent on input from the following deliverables: D1.1.6, D1.2.3.



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Task 2.3: New transfer standards (CETIAT, INRIM, TUBITAK)

(Start Jun 13, End Jan 16)

The aim of this task is to develop improved methods and equipment for the transfer standard based dissemination of SI traceability. To achieve this, two approaches will be followed:

1. Development of a non-invasive and non-destructive transfer standard based on radio-frequency wave and microwave at a low energy level (0 dBm / few mW) for direct determination of moisture.

2. Development of a low-cost, portable system comprising a microwave moisture meter and a system for maintaining an internal reference in very stable conditions. Due to the versatility with respect to the internal reference and the microwave measurement, the system will be applicable to a wide range of materials and applications.

Because the relaxation frequency of the water in a material depends on the degree of binding of the water, the first approach leads to a transfer standard capable of providing information on the water binding. Although this measurement principle has been known since the 1970s, it has never been applied to a moisture measuring instrument working in a wide frequency range with a capability of detecting the degree of binding of water in the sample.

The major components in a system based on the second approach are well known and widely used but they have never been combined into a single set-up to provide dissemination of traceability in moisture measurements. In addition, novel developments are needed to obtain the required versatility.


Following the first approach, CETIAT will develop a RF/MW transfer standard instrument which allows scanning over a wide range of frequencies from radio-frequency (RF) waves up to microwaves (MW) and a wide range of moisture, nominally 10 g/kg to 950 g/kg. The system will consist of a set of 4 or 5 resonant or non resonant coaxial cells, allowing working with a wider range of frequencies than waveguide-type cells. A paper will be written. (CETIAT) (D2.3.1, D2.3.2, D2.3.3, D2.3.4)

Following the second approach, INRIM will design and construct a microwave moisture meter and a portable humidity generator. The system will satisfy requirements of 1) versatility, with regard to the characteristics (material, shape, density) of the moist sample under test, 2) modularity, allowing fast interchangeability of sample holders, 3) portability, to facilitate its use as a part of a transfer standard. These requirements are envisaged in a conductive cavity (e.g. a cylinder) comprised of elements which are easily replaceable with the sample holder(s) developed in Task 2.2. The modularity of the design will allow for implementing more than a single measurement method (dielectric or conductive resonator, waveguide), enhancing the range of operating frequencies and measurable permittivities. Outcomes of the modelling development in WP3 will be exploited in analysing the effect of moisture gradients and interaction between the specimen and the instrument under calibration. (INRIM) (D2.3.5, D2.3.6, D2.3.7, D2.3.8)

Using cKF and LoD methods, TUBITAK will carry out reference measurements for selected materials to be used in tests for the transfer standards. (TUBITAK) (D2.3.9)

Major facilities to be used: none

This task is dependent on input from the following deliverables: none.


The deliverables of this task are required for tasks: 1.3, 3.2, 3.3.

Task 2.4: Novel calibration methods for surface moisture sensors (UL, CMI, TUBITAK)

(Start Mar 14, End May 16)

The aim of this task is to develop traceable calibration methods and facilities for surface moisture sensors. The traceability is obtained through determination of a controlled moisture gradient in a specimen.

Two different set-ups will be developed specifically for polymer elements and plastic/paper specimens, respectively, according to the interests expressed by industrial stakeholders. Because of similarities between the set-ups, the methods can be validated by comparing them with each other.

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UL will design and construct a calibration system for sensors measuring surface moisture in polymer elements. Moisture gradients will be controlled and determined by introducing moisture transport through a polymer specimen with separate controlled humidity environments on each side of the specimen. The moisture of the specimen will be determined from humidities on both sides of the specimen, the linear moisture gradient across the specimen, and the sorption isotherm of the specimen. The sorption isotherm will be determined in a humidity controlled chamber using a chilled mirror hygrometer and a TGA as the references for humidity and moisture content. The controlled humidity level will range up to 80 % rh. As a final stage of the development, UL will carry out an uncertainty analysis comprising all relevant sources of uncertainty. Outcomes of the modelling development in WP3 will be exploited in analysing the effect of moisture gradients and interaction between the specimen and the instrument under calibration. (UL) (D2.4.1, D2.4.2, D2.4.5)

TUBITAK will develop a calibration system for surface moisture meters for paper/plastic specimens, including uncertainty analysis. Both TGA and cKF will be used for bulk moisture determinations. Moisture gradients will be controlled by controlling ambient air humidity and moisture in the base of the specimen. (Surface moisture meters will be supplied by an industrial collaborator, Metso). (TUBITAK) (D2.4.3, D2.4.4, D2.4.5)

UL and TUBITAK will carry out a comparison with a polymer specimen. (UL, TUBITAK) (D2.4.5)

To underpin the calibration system development at UL, CMI will measure the effect of different humidity conditions on the thermal conductivity of a polymer element. One side of the specimen will be exposed to a dry environment, while the other side to changing levels of humidity (10 % rh to 90 % rh), which will be measured by a precision dew-point meter. (CMI) (D2.4.5)


This task is dependent on input from the following deliverables: D1.1.7.



C2.b Labour Resources for WP 2

1- M

IKE

S

2- B

RM

L

3- C

ETIA

T4-

CM

I

5- D

TI

6- IN

RIM

7- N

PL

8- T

UBIT

AK

9- U

L

10- U

T

11- R

EG

(UN

ICLA

M)

TO

TA

L

WP2 7.0 9.5 13.0 10.0 11.0 12.5 7.0 11.6 2.0 83.6

C2.c Summary of Deliverables for WP 2

Deliverable number


Other Participants

Deliverable type

Delivery date

2.1.1 The list of candidate materials prepared

NPL BRML, UT Report May 14

2.1.2 Uncertainty analysis data for at least one CRM

NPL BRML, UT Data Jan 15

2.1.3 At least one new CRM available NPL BRML, UT Artefact Sep 15

2.2.1 Review report on procedures relevant to transportation of samples and CRMs

BRML Report May 14

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2.2.2 Submission of peer-reviewed journal or conference paper on the RH/T logger based sample monitoring method to quantify the effect of transportation on the stability of processed wood and biomass samples

MIKES Publication Jul 15

2.2.3 Submission of peer-reviewed journal or conference paper on the effect of ambient conditions and packaging on the stability of wooden samples during transportation

CMI MIKES Publication Mar 15

2.2.4 At least 3 sample holders designed and tested

INRIM Artefact Sep 14

2.2.5 Submission of peer-reviewed journal or conference paper on the effect of ambient conditions and packaging on the stability of food and pharmaceutical powders and paper samples during transportation

BRML TUBITAK Publication Nov 14

2.2.6 Report on potentiality of applying a correction factor to reduce the effect of transportation

MIKES CMI Report Aug 15

2.2.7 Good practice guide for estimating the uncertainty due to sample handling and transportation

CMI BRML, MIKES, TUBITAK

Good Practice Guide

Sep 15

2.3.1 Design of resonant or non resonant coaxial cells for RF/MW transfer standard instrument

CETIAT Design May 14

2.3.2 At least 4 resonant or non resonant coaxial cells ready

CETIAT Device Nov 14

2.3.3 Complete RF/MW transfer system with initial tests

CETIAT Device Mar 15

2.3.4 Conference report or publication on the transfer standard using microwaves and radio frequencies approach and its validation

CETIAT Publication Sep 15

2.3.5 Microwave moisture meter INRIM Device Nov 14

2.3.6 Portable humidity generator INRIM Device Mar 14

2.3.7 Complete transfer standard system with initial tests

INRIM Device Sep 15

2.3.8 Conference report or publication on transfer standard system comprising MW moisture meter and a portable humidity generator

INRIM Publication Jan 16

2.3.9 Reference measurements for transfer standards tests

TUBITAK Dataset Jan 16

2.4.1 Design of a calibration system for sensors measuring surface moisture in polymer elements

UL Design May 14

2.4.2 Complete system with initial tests UL Device May 15

2.4.3 Design of calibration system for sensors measuring surface moisture in plastic/paper elements

TUBITAK Design May 14

2.4.4 Complete system with initial tests TUBITAK Device May 15

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2.4.5 Report on validation of calibration methods for surface moisture meters including uncertainty evaluations

UL TUBITAK, CMI Report May 16

C3 WP3: Metrological underpinning for moisture

(INRIM, CMI, DTI, UL, TUBITAK, UT, REG(UNICLAM), BRML)


Aim

The aim of this workpackage is to underpin new traceability mechanisms and to improve the applicability of existing SI traceability mechanisms for moisture using validated mathematical modelling including uncertainty models for moisture measurements. These need to address issues such as moisture transport in materials, bulk moisture, surface properties and moisture profile. Underpinning the traceability mechanisms to be developed in WP1 and WP2 will comprise: 1) the development of modelling relevant to moisture metrology, both in steady-state and transient regimes (Task 3.1), 2) the experimental validation of models in selected cases and the investigation, through numerical modelling, of the interaction of measurand with measuring instrument (Task 3.2), and 3) the analysis of the uncertainty sources, both of models and measurement processes, in order to build up comprehensive model uncertainty budgets applicable to practical cases of interest for accredited testing and calibration laboratories and accreditation bodies and others (Task 3.3).

Background

The physics of moisture in materials is a highly non-linear process which combines mass and energy transfer with phase transitions within porous media. Once ab/adsorbed in the porous structure, the process can be described in terms of increasing binding energy levels such as: 1) free water, on the surface of the substance, 2) physically-bound capillary water, in pores and at heterogeneous joints, 3) physico-chemically absorbed water, 4) chemically-bound water. The vapour phase can also be present in equilibrium with the liquid phase.

Most moisture measurement methods are unable to detect the range of binding energies associated with absorbed water but knowledge of these can help to gain insight into material properties, such as mechanical strength, dimensional stability and thermal performance. Furthermore, the transient behaviour of moisture-related phenomena and the influence of surface moisture and moisture transport/diffusion on measuring instruments and measurement methods requires a detailed knowledge of temperature, pressure, velocity and species concentration in the physical domain under investigation (e.g., at the surface, in the bulk, or at the boundary layer). Such knowledge can be gained by developing a suitable detailed mathematical description of both free-fluid and porous regions in non-stationary conditions. Once such a model (analytical or numerical) is available, it can act as a “virtual laboratory” to assist in the design of moisture control systems (e.g. in drying processes), in the determination of the optimal moisture conditions for a given material (e.g. in CRM development and storage), and in the investigation of the interaction between moist samples and moisture content measurement methods (e.g. for instrumentation development).

In moisture measurements, variables such as sample collection, handling, transport, and storage influence results before any measurement has been carried out. The interaction between the measurand and the measuring instrument is another not negligible source of error. When standardised procedures are followed, their impact and the resulting measurement errors may be minimised. Common practice in physical measurements is to focus on the uncertainty in the measuring process, but a thorough uncertainty analysis should include the whole process from sampling until reporting. With all uncertainties quantified and presented together in tabular or spreadsheet form as an uncertainty budget, a laboratory will have a tool to identify the (most) relevant uncertainty sources for each specific case. With a systematic approach the magnitude and probability distribution function of the different uncertainty sources can be estimated and, whenever possible, the overall uncertainty can be minimised by focusing on the sources that contribute most to the combined uncertainty.

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The objectives and research methodology of this WP are summarised in the figure below:

Metrological

underpinning

for moisture

Task 3.1

develops physical

and empirical

models for

moisture

transport and

profile (bulk and

surface).

Task 3.2 performs experiments to

validate the models and investigate

the interaction between measurand

and instrument.

Task 3.3 develops

comprehensive

tools targeted to

estimating

uncertainty in

moisture

measurements

and calibrations.



Task 3.1: Modelling (INRIM, CMI, DTI, TUBITAK, REG(UNICLAM))

(Start Jun 13, End May 15)

The aim of this task is to develop physical and empirical models and thus achieve a fundamental understanding of the physical processes during moisture transport in selected materials including effects like surface moisture and moisture profile. The developed engineering computer models can then be used to simulate the moisture transport in the materials in different operating conditions as well as to contribute to the definition of the measurand, i.e. a better understanding of the measurement for a better uncertainty estimate.


INRIM and REG(UNICLAM) will develop a mathematical model able to describe free-fluid and porous regions in selected materials, both in steady-state and transient regimes. The heat and mass transfer with phase change in wet porous media will be modelled through the liquid and vapour mass, momentum and energy conservation equations with the addition of the capillary transport of liquid and the diffusion of water in the thickness direction. Also the effect of transient variation of physical proprieties as the thermal conductivity, the vapour and liquid diffusivity due to the liquid accumulation on the dynamic behaviour will be considered. The results of this work will be included in a paper on mathematical modelling of moisture processes. (INRIM, REG(UNICLAM)) (D3.1.1, D3.1.4)

To underpin the numerical modelling, CMI will develop a mathematical model of temperature distribution on the surface and inside of the materials in both steady and dynamic states. CMI will investigate material properties such as thermal conductivity and emissivity both numerically and experimentally. (CMI) (D3.1.2)

REG(UNICLAM) will develop a generalised-model approach based on partially porous domains. The numerical model and code will rely on algorithms based on the so-called Artificial Compressibility Characteristic-Based Split (AC-CBS) developed by the REG-Researcher and adapted to study such phenomena. A fully numerical tool – validated against experiments in Task 3.2 – will be developed in order to estimate the moisture profile in selected materials (such as non-woven fibres, polymers or pharmaceuticals) and to investigate its dependence from material properties and state (such as thickness, vapour permeation and thermal/moisture exchange rate at the surface). A paper will be written on the modelling. (REG(UNICLAM)) (D3.1.3, D3.1.4)

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DTI will develop physical and empirical models for selected materials to extend the monitoring capabilities of in-situ moisture sensors. The effects of an uneven moisture distribution in the product or in the bulk will be accounted for in the models which thereby can be used to reduce the measurement uncertainty. Depending on the material properties, structure and processing conditions, different physical models describing internal water transport in the product can be used. Simpler diffusional models will be used in some cases; otherwise the internal pressure build-up in the material may warrant use of advanced models including accounting for vapour transport and capillarity effects. The results obtained from this activity will feed into Task 1.1. (DTI) (D3.1.5)

TUBITAK will develop a mathematical model to describe diffusion of moisture in paper sheet material in order to improve the knowledge of measurement errors in thin sheet materials relevant to uncertainty measurement analysis. (TUBITAK) (D3.1.6, D3.1.4)

REG(UNICLAM) will separately verify and validate different aspects of the mathematical and numerical models. Such an objective will be reached by selecting representative numerical and analytical benchmarks available in the scientific literature. Results from the numerical model will be compared with experimental data available in the literature regarding moisture related problems and DTI will provide input. (REG(UNICLAM), DTI) (D3.1.7)


This task is dependent on input from the following deliverables: D2.4.3.



Task 3.2: Selected experimental validation of models (CMI, INRIM, DTI, TUBITAK, UL, REG(UNICLAM))

(Start Mar 15, End May 16)

The aim of this task is two-fold: 1) to design and perform experiments with selected materials in order to validate the mathematical models and the associated computer software tools for moisture metrology developed in Task 3.1, and 2) to investigate, through numerical modelling, the interaction between the measurand and the measuring instrument in order to support instrument development in Task 2.3. The surface moisture calibration facilities will also be part of this effort.


INRIM and REG(UNICLAM) will design one or more experiments suitable for validating the analytical and numerical models concerning moisture profile and moisture transport/diffusion in selected materials, such as non-woven fibres, polymers, and/or pharmaceuticals. (INRIM, REG(UNICLAM)) (D3.2.1)

INRIM and REG(UNICLAM) will set up at least one experiment with suitable CRMs, made available from Task 2.1, in order to validate the numerical tools, including their ability to predict the effect of influence parameters and the associated model uncertainty. (INRIM, REG(UNICLAM)) (D3.2.2)

UL will set up at least one experiment in conjunction with Task 2.4 with a suitable polymeric element in order to validate the numerical model for surface moisture measurement. (UL) (D3.2.1, D3.2.2)

UL and INRIM will separately investigate – through modelling and experiments – the interaction between the measurand and the measuring instrumentation. This will be an integral part of the validation of the calibration method for surface moisture at UL and the microwave transfer standard system for bulk moisture at INRIM (both developed in WP2). A paper will be written on the results. (INRIM, UL) (D3.2.3, D3.2.4, D3.2.5)

Applying modelling and appropriate experiments, CMI will investigate the impact of thermal effects and local temperature distribution – at the surface and in the bulk – on moisture content measurements. This will contribute to a better definition of the allowable ranges of variability and threshold of such parameters in a practical measurement context, and allow for operation and storage of the CRMs in optimal conditions in order to achieve and maintain consistent performance over time. The results of this activity will be included in the paper on the interaction between the measurand and the measuring instrumentation. (CMI) (D3.2.6, D3.2.5)

REG(UNICLAM) will test the modelling software tool with DTI and TUBITAK, using experimental data from selected measurement cases. (REG(UNICLAM), DTI, TUBITAK) (D3.2.7)

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Major facilities to be used: UL: calibration system for surface moisture meters developed in WP2, Mettler Toledo moisture analyser HX204, INRIM: transfer standard system for moisture developed in WP2.

This task is dependent on input from the following deliverables: D2.1.3, D2.3.5, D2.4.2, D3.1.2, D3.1.3.



Task 3.3: Model uncertainty analysis (TUBITAK, BRML, INRIM, UT, REG(UNICLAM))

(Start Nov 15, End Mar 16)

The aim of this task is to develop a comprehensive tool for estimating uncertainty in moisture measurement processes. Several model uncertainty budgets that include both continuous and discrete uncertainty sources will be set up for selected case studies. A single uncertainty budget will include all the influence parameters for the measurand as identified in Tasks 3.1 and 3.2 and in WP2. The task will be targeted to quantify uncertainties and to present case studies in spreadsheet form. Therefore, this WP will provide an excellent tool for optimising the quality of measurements and for underpinning measurement best practices in testing and calibration laboratories as well as in industrial process applications.


INRIM and REG(UNICLAM) will carry out an analysis of the uncertainty sources related to moisture profile and moisture transport in selected materials (such as non-woven fibres, polymers or pharmaceuticals) by using the estimates from the numerical model developed in Task 3.1 and its validation in Task 3.2. (INRIM, REG(UNICLAM)) (D3.3.1)

TUBITAK and BRML will develop a comprehensive analysis of the uncertainty sources deriving from sampling, collection, handling, transport and storage of moist paper samples, as identified in Task 2.2. Each of the uncertainty sources will be studied separately by paired observations between a standard method and an alternative approach developed in WP2. (TUBITAK, BRML) (D3.3.2)

INRIM will develop a set of model uncertainty budgets for selected case studies in spreadsheet form that will include both continuous and discrete uncertainty sources and the associated probability distribution functions. (INRIM) (D3.3.3)

BRML and UT and TUBITAK will carry out uncertainty analyses of moisture measurements applied to specific measurement problems selected from amongst those relevant for accredited testing and calibration laboratories. (BRML, TUBITAK, UT) (D3.3.3)


This task is dependent on input from the following deliverables: D1.1.7, D1.2.1, D1.2.5, D2.2.5, D2.3.7.




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Deliverable number

Deliverable description Lead Participant Other Participants

Deliverable type

Delivery date

3.1.1 (REG D1.2)

Mathematical modelling of moisture processes in selected materials

INRIM REG (UNICLAM)

Report Feb 14

3.1.2 Model of temperature distribution

CMI Report Aug 14

3.1.3 (REG D1.3)

Numerical model and code to investigate time-dependent moisture and thermal profile in selected materials

REG(UNICLAM) Software tool May 14

3.1.4 Submission of peer-reviewed journal or conference paper on mathematical modelling of moisture processes

INRIM TUBITAK, REG (UNICLAM)

Publication Nov 14

3.1.5 Report on modelling of mass transfer in drying of selected materials and how this affects an inline moisture sensor

DTI Report Nov 14

3.1.6 Model for diffusion of moisture in paper sheet

TUBITAK Model Nov 14

3.1.7 Report on model verification REG(UNICLAM) DTI Report May 15

3.2.1 (REG D3.1)

Report on design of experiments for modelling validation

INRIM UL, REG (UNICLAM)

Report Jul 15

3.2.2 (REG D3.2)

Report on validation of numerical tools for moisture models


Report Sep 15

3.2.3 Report on validation of the calibration method for surface moisture

UL Report Nov 15

3.2.4 Report on validation of microwave measurement method for bulk moisture

INRIM Report Aug 15

3.2.5 Journal or conference paper on interaction between the measurand and the measuring instrumentation in moisture metrology submitted

INRIM CMI, UL Publication Nov 15

3.2.6 Report on impact of thermal effects and local temperature distribution on moisture content measurements

CMI Report Aug 15

3.2.7 (REG D3.4)

Report on the application of the modelling software tool

REG(UNICLAM) DTI, TUBITAK Report May 16

3.3.1 (REG D3.3)

Report on uncertainty analysis of numerical modelling

INRIM REG (UNICLAM)

Report Mar 16

3.3.2 Report on uncertainty evaluations for moisture measurements in paper

TUBITAK BRML Report Mar 16

3.3.3 Model uncertainty budgets based on spreadsheet form targeted to calibration and testing laboratories

INRIM BRML, TUBITAK, UT

Software tool Mar 16

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C4 WP4: Creating Impact

(NPL, BRML, CMI, CETIAT, DTI, INRIM, MIKES, UL, TUBITAK, UT, REG(UNICLAM))

Start month: Jun 13, End month: May 16

The aim of this workpackage is to ensure the benefits of the project are realised through dissemination of the technical outcomes to stakeholders at all levels, and by developing and strengthening the metrology infrastructure in the moisture field.

Knowledge transfer activities will include liaison with stakeholders in group activities and individually (through meetings, visits, correspondence, and though collaborative inputs into technical tasks). The JRP will provide an informative website, scientific presentations and publications, user-friendly good-practice guides, and a strong expansion of new contacts into a large number of relevant standardisation committees.

New training material will be developed covering best practice in moisture metrology, measurement traceability, and uncertainty. This material will be available to all JRP-Partners to adapt for delivery at any level from NMI scientists to industrial end-users of measurements, translated into local languages if required.

Metrology infrastructure is the subject of a specific task in order to bring coherence to what are currently rather fragmented processes. This will intensify the focus of JRP-Partners’ existing activities at CC, RMO, and other levels, bridging chemical and physical metrology, and delivering a step change in the achievement of the goals of these co-operations.

Exploitation of the project outputs will include the provision of new or improved measurement services or consultancies to customers, on commercial terms, by most of the JRP-Partners.

Because published standards are strongly influential in moisture measurement and calibration practices, standardisation committees are a particularly important target. The standards can be improved by the inclusion of traceable calibration methodology, and this in turn has enormous potential to impact end-users of moisture measurements across many and varied sectors. Hence, working with the standards-writing community is vital to achieving the aims of the JRP.

Existing memberships and links to committees and technical working groups include:

EURAMET: TC-T (SC Humidity, WG Best Practice, WG Strategy); TC-MC and TC-M

CIPM Consultative Committees:

o CCT: including WG6 Humidity measurements, WG7 key comparisons, WG9 thermophysical properties and WG-S Strategy

o CCQM: including OAWG, IAWG, and WG on Grain Moisture

IMEKO TC12 Temperature and thermal measurements

NCSL International

National and international standardisation committees or mirror groups of these, including: CEN/TC 335 Biofuels; CEN/TC 346 Conservation of Cultural Heritage; CEN/TC 89 (thermal isolation); CEN/TC 112/TC 124/TC 175 (wood); IEC TC 38 Instrument transformers; IEC TC65 Industrial-process measurement, control and automation; IEC SC65B Measurement and control devices; OIML TC17/SC1 Humidity; BSI CPI 29 Humidity and temperature conditioning requirements.

A number of national user interest groups such as National Kelvin Club (Finland), Measurement Network (UK).


Task 4.1 Knowledge transfer (NPL, All JRP-Partners))


The aim of this task is to share the research findings of the JRP with the wider community. It includes knowledge transfer both to and from stakeholders, especially those who have requested to formally collaborate in the JRP.

Knowledge transfer will be firstly (but not only) with enlisted supporters of the JRP. These include NMIs across all RMOs (many with well-established moisture activity), chairs of technical working groups,

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accredited testing and calibration laboratories, suppliers of moisture instrumentation and drying equipment, commercial research organisations, university research departments, and of course companies manufacturing moisture-critical products. The direct interests of these stakeholders include chemicals, pharmaceuticals, polymers and plastics; adhesives; paper; wood; foodstuffs and animal feeds; solid biofuels; and related raw materials or finished products. During the JRP, the knowledge transfer activities will reach and engage further organisations and sectors.


Liaison with stakeholders through two-way sharing of information, by correspondence, meetings, visits, and other actions – including input from them into the JRP work, by advising on technical details and user needs. Stakeholders will be informed about JRP progress via the website and by e-mailed updates on the work. They will be able to participate in JRP workshops, and some of them will be target audiences for training. Existing EURAMET Project 1065, on moisture measurement and strategy, is open to all EURAMET members and associates, and offers a unique route of engagement for this group. (MIKES, all) (D4.1.1)

A JRP website. This will be set up by UL, who will design and maintain the site, with content management allowing inputs of JRP-Partners. The regularly updated (at least every six months) content will include an overview of the project, contact details, key events, and other information as the work progresses. A domain name (metef.net) has already been registered. (UL, all) (D4.1.2)

Interaction with standardisation committees. JRP-Partners will channel information and influence standards in the course of their existing participation in moisture-related standardisation committees. Outreach into further areas of standardisation will be made by newly approaching relevant committees at active times (during revision or public draft stage of standards) and offering input on moisture calibration, traceability and uncertainty. At least 20 standards committees will be newly approached on a rolling timescale during the project (EN/ISO committees directly, or through national bodies), prioritising those standards to which moisture is critical. A by-product will be the awareness and involvement of a large diverse set of moisture experts in the JRP. (NPL, INRIM, DTI) (D4.1.3)

Standards Committee / Technical Committee / WG

JRP-Participants involved

Likely area of impact / activities undertaken by JRP-Participants related to standard/committee

CEN/TC 335 Biofuels DTI

National delegate will promote awareness of the JRP; channel information to/from the committee; channel advice and best practice, where expertise from the JRP can influence development or updating of a standard, specifically on calibration, measurement traceability, and measurement uncertainty for moisture in materials.

CEN/TC 346 Conservation of Cultural Heritage

INRIM

CEN/TC 89 (thermal isolation) DTI

CEN/TC 112/TC 124/TC 175 (wood) DTI

IEC TC 38 Instrument transformers INRIM

IEC TC65 Industrial-process measurement, control and automation

INRIM

IEC SC65B Measurement and control devices

INRIM

BSI CPI 29 Humidity and temperature conditioning requirements

NPL

Further committees will be identified for targeting (from the review in Task 1.1), selected for maximum relevance or impact

NPL Depending on the stage of each standard in its development or review cycle, JRP-Partner will newly approach committee chairs, or national delegates, or will input to drafts at public comment stage, specifically on calibration, measurement traceability, and measurement uncertainty for moisture in materials.

Publications in conventional and electronic (online) media, spanning trade magazines, peer-reviewed scientific journals, both sector-specific and measurement journals. Likely target journals include Metrologia, Measurement Science and Technology, Review of Scientific Instruments, Analytical Chemistry, Journal of Physical Chemistry, Drying Technology, and Surface and Interface

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Analysis. Proposed sector and trade magazines include Plus Proces, and Measurement+Control. This will comprise at least 5 publications submitted during the course of the JRP. In addition other publications are shown as deliverables within technical WPs. (DTI, BRML, CETIAT) (D4.1.5)

Presentations at conferences. JRP-Partners will deliver at least 5 presentations, covering an overview or individual deliverables of the JRP, at leading international conferences and other relevant fora during the course of the JRP. Target conferences include International Symposium on Humidity and Moisture (date to be announced – approx. 2015), EuroFoodWater 2014 and 2016, TEMPMEKO 2016, International Metrology Congress (October 2013, 2015), NCSLI Conference 2014, Annual International Conference on Lyophilisation and Freeze Drying, and numerous possible sector-based conferences. Presentations will also be made to relevant EURAMET audiences at annual TC meetings. (MIKES, BRML, CETIAT, DTI, NPL, REG(UNICLAM)) (D4.1.4)

Best-practice guides. Two guidance documents will be developed that describe best practice of traceable measurement and testing methodology. These will be made available to download for distribution in electronic form.

Guide on industrial sampling and sample handling, in concise format targeted at industry users needing calibration services (developed from WP2, D2.2.7).

Guide for laboratories on the usage of coulometric KF titration and on evaluating the uncertainty of coulometric KF titration. (UT, DTI) (D4.1.6)


Task 4.2 Training (CETIAT, DTI, INRIM, MIKES, TUBITAK, UT, REG(UNICLAM))

(Start Nov 13, End May 16)

The aim of this task is to enable the knowledge acquired in the JRP to be disseminated though training which will promote best practice in moisture measurement. Training material will be developed during the project, for use by JRP-Partners within and beyond the time frame of the project. JRP-Partners will be free to adapt the material for widespread delivery to different levels of audience, and to translate it for accessibility in local languages. Target audiences will range from industrial and laboratory measurement users, to university students, to NMIs (such as those in EURAMET countries aiming to develop moisture metrology capabilities). The training content will include moisture measurement techniques, measurement traceability, and uncertainty evaluation, as well as case studies for selected examples of practical measurements.


Training material covering moisture measurement techniques, measurement traceability, and uncertainty evaluation will be developed and made available in the form of PowerPoint presentation files to JRP-Partners. (CETIAT, DTI, UT) (D4.2.1)

The developed training material will be presented by JRP-Partners in at least two training events during the JRP. The target audience size will be at least 10 trainees per event.

Case-studies or examples on determination of water content will be introduced into the teaching materials of existing training and study programmes: (1) TrainMiC http://www.trainmic.org/); (2) Applied Measurement Science (http://www.ut.ee/ams/), (3) Measurement Science in Chemistry (http://www.msc-euromaster.eu/).

At least four workshops will be held by JRP-Partners for the benefit of measurement stakeholders. Workshops will take the form of seminar-style events with multiple speakers on a range of moisture topics, which may combine scientific reporting and training elements, including best practice disseminated from the JRP. The target audience size will be at least 20 attendees per workshop. (CETIAT, INRIM, MIKES, TUBITAK, REG(UNICLAM)) (D4.2.2)

REG(UNICLAM) will provide training to DTI in mathematical modelling and DTI will provide training to REG(UNICLAM) in moisture measurements. (D4.2.3)


http://www.trainmic.org/

http://www.ut.ee/ams/

http://www.msc-euromaster.eu/

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Task 4.3 Metrology infrastructure building (NPL, all)


The aim of this task is to enhance the national and international metrological structures supporting moisture metrology, and promote effective cross-disciplinary cooperation among these, so as to provide a clear metrological framework in the moisture field, to meet industrial and societal need. This task will particularly extend the influence of the project well beyond the JRP-Partners to wider Europe and worldwide.

This task is in addition to, and distinct from, general stakeholder liaison (which will focus on techniques and practices) whereas metrology infrastructure building will address the entire organisational framework for moisture metrology, nationally and internationally.

Across EURAMET, a multi-level development can be envisaged in the moisture field, broadly comprising “NMI centres of excellence”, “national moisture facilities”, and the option of devolved provision through EURAMET traceability agreements. The sharing of JRP progress and outputs, as well as the training developed in Task 4.2, will support capacity-building for NMIs to any required level. Accreditation bodies and their practices are also a target area for impact as part of the overall metrology infrastructure.

Progress and outcomes will be reported during the course of the JRP, and in addition there will be steps towards longer-term goals beyond the time frame of the project.

Specific focal points for interaction include annual EURAMET TC meetings, existing EURAMET project 1065 Survey and strategic planning in the field of measurement of moisture in materials, meetings of CCQM working groups (IAWG, OAWG), and meetings of CCT WG6 (expected 2014 and 2016).


JRP-Participants and collaborators, though their existing memberships and chairmanships, will actively promote the goals of the JRP in national and international working groups at CC, RMO, IMEKO and other fora concerned with metrology infrastructure for moisture. (NPL, all) (D4.3.1)

JRP-Participants will form new cooperations, with NMIs and DIs with developing or well-established moisture standard provision, not only in wider EURAMET, but also globally where there are pockets of considerable NMI expertise. Interest has already been expressed by NIST (USA), PTB (Germany), KRISS (Korea), NMC A-STAR (Singapore), MSL (New Zealand), UNIIM (Russia), VNIIM (Russia), INTI (Argentina) and a number of African NMIs.

Cooperations will be strengthened between centres of moisture expertise bridging between disciplines of physical and chemical metrology (for example between CCT and CCQM, EURAMET TC-T and TC-MC, and nationally between NMIs and DIs where physical and chemical metrology are not co-located).

Inter-NMI traceability agreements will be offered by relevant JRP-Partners (formalised as EURAMET projects, for example) for those EURAMET countries requiring moisture services without themselves developing capability.

Steps will be taken to identify and propose key comparisons needed in the moisture field, considering requirements already under discussion (for example grain moisture in CCQM) as well as possible comparisons testing broader moisture capabilities not tied to a specific material.

Proposals will be made for how to address moisture CMC claims and reviews, aiming to prepare CMCs for moisture, for submission to the BIPM database.

Relevant developments from the JRP on moisture methods, traceability, comparisons and CMCs will be shared with accreditation bodies (EA, ILAC, national schemes) and with cooperating laboratories accredited for moisture activities. This will be designed to promote best practice in moisture measurement traceability in the accreditation context.

JRP-Partners will maintain interaction with aspects of the legal metrology framework for moisture, where appropriate.

Further recommendations for action beyond the time frame of the JRP will be summarised in the deliverable report D4.3.2. (NPL, all) (D4.3.2)


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Task 4.4 Exploitation (NPL, BRML, DTI, INRIM, MIKES, TUBITAK, UT)

(Start Nov 14, End Apr 16)

The aim of this task is to provide for the exploitation of the project outputs. A number of JRP-Partners will develop new commercial measurement, calibration or testing services; or new reference materials or artefacts; or become able to offer these commercial products and services with improvements in scope, methodology, or uncertainty. In addition, the use of project outputs in new or revised published standards is a form of exploitation covered in Task 4.1.

There is scope for knowledge generated in the project to provide other intellectual property benefits for the originating JRP-Partners. The usual provisions of IP agreement will be made at JRP-Contract stage. The further potential for commercialisation of results will be considered as work progresses.

The JRP-Partners are already aware of the possibilities for further moisture-related research to be funded through European Framework Programmes. It is noted that, whereas the EMRP can uniquely address SI metrology, European FPs normally call for research focused on particular industries or sectors – where there are numerous applications for improved moisture metrology.


New or improved measurement, sampling and calibration services, focusing on provision of fully traceable measurement and calibrations, using methods developed and validated in the project. This will include a new service type: in-situ sampling for calibration. (BRML, DTI, MIKES, NPL, TUBITAK) (D4.4.1)

Improved or extended consultancy services, advising on techniques for moisture, but especially on traceability and uncertainty in moisture measurements. Consultancy will be especially targeted at areas such as drying technology, and testing and calibration laboratories, which have wide reach across many sectors; but also targeting key industries in particular regions. (INRIM, DTI, MIKES) (D4.4.2)

Exploitation plan for new certified reference material(s) developed in the project, identifying potential markets, manufacturers, and distributors, and considering any IP and commercial prospects. (NPL, BRML, UT) (D4.4.3)



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Deliverable number


Other Participants

Deliverable type

Delivery date

4.1.1 Liaison with stakeholders though two-way sharing of information, by correspondence, meetings and visits

MIKES All Reports May 14, May 15, May 16

4.1.2 Registration, design, and maintenance of website with content management allowing inputs of JRP-Partners, updated every 6 months

UL All JRP web site Aug 13, Nov 13, May 14, Nov 14, May 15, Nov 15, May 16

4.1.3 Active input and dissemination though sector technical and standards committees

NPL INRIM, DTI Reports May 14, May 15, May 16

4.1.4 At least 5 presentations at conferences, presenting overview or individual outputs of the project

MIKES BRML, CETIAT, DTI, NPL, REG (UNICLAM)

Conference presentations

May 14, Nov 14, Sep 15, Nov 15

4.1.5 At least 5 paper or electronic publications spanning trade magazines, sector-specific and measurement journals

DTI BRML, CETIAT

Publications

May 14, May 15, Apr 16

4.1.6 Guide on Karl-Fischer titration usage and uncertainty evaluation

UT DTI Good practice guide

Sep 15

4.2.1 Develop new training course material and case studies

CETIAT DTI, UT Progress report

Training course material

Nov 14

Apr 16

4.2.2 Workshops including scientific reports of the project and/or training elements

CETIAT INRIM, MIKES, TUBITAK, REG (UNICLAM)

Workshops Nov 14, May 15, Nov 15, May 16

4.2.3

(REG D4.6)

2-way training during Guestworking REG(UNICLAM) DTI Training Apr 15

4.3.1 Two-way liaison with relevant groups in IMEKO, EURAMET and other RMOs, and relevant CIPM CCs

NPL All Reports May 14, May 15, May 16

4.3.2 Report proposing future actions on international metrological infrastructure for moisture metrology

NPL All Report Mar 16

4.4.1 New/improved calibration, sampling and measurement services

BRML DTI, MIKES, NPL, TUBITAK

Progress report

Service

Nov 14

Mar 16

4.4.2 Extend upon existing consulting services

INRIM DTI, MIKES Consultancy service

May 15

4.4.3 Report on the exploitation route for new CRM(s) developed during the project

NPL BRML, UT Report Apr 16

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C5 WP5: JRP Management and Coordination

(MIKES, BRML, CMI, CETIAT, DTI, INRIM, NPL, UL, TUBITAK, UT, REG(UNICLAM))

Start month: Jun 13, End month: May 16

The aim of this WP is to provide well-structured and efficient management and coordination for this JRP. This will be realised through active overall management by the JRP-Coordinator, efficient WP management by the WP leaders, regular project meetings and regular reporting.

A Project Management Board (PMB) will be established consisting of the JRP-Coordinator and the WP Leaders. The PMB will be responsible for the strategic direction of the project, and resolving any disputes within the JRP-Consortium. The PMB will continuously monitor the progress in the JRP and initiate actions if new challenges or discrepancies from the project plan are identified or foreseen. The PMB will be chaired by the JRP-Coordinator.

The JRP-Coordinator is the reference point for the JRP-Participants and EURAMET e.V.


Task 5.1: JRP and REG management (MIKES, all)



The JRP-Coordinator will carry out the day-to-day overall management of the JRP.

The WP leaders (MIKES/WP1&WP5, CETIAT/WP2, INRIM/WP3 and NPL/WP4) will coordinate the work in their WPs.

As the JRP-Coordinator and WP leaders, the representatives of MIKES, CETIAT, INRIM and NPL will be the members of the PMB. This Board will have internet or face-to-face meetings at least twice a year.

The REG-Researcher located at Università degli Studi di Cassino e del Lazio Meridionale (Cassino, Italy) has strong links with the WP3 leader INRIM who will supervise progress with and aid planning of the technical work.

REG(UNICLAM) will attend all JRP meetings, and will report according to the same schedule as the other JRP-Partners, and fulfilling the deliverables in the EMRP Researcher Grant Contract. He will report technical progress to INRIM (WP3 leader), impact to NPL (WP4 leader) and management to MIKES (JRP-Coordinator). All reports will be copied to the JRP-Coordinator.

Task 5.2: Project meetings (MIKES, all)



A Kick-off meeting will be held at the inception of the project (minimum duration 2 days). The meeting will be organised and hosted by MIKES. The kick-off meeting will ensure that all JRP-Participants are clear as to the objectives of the project and their contribution to it. It is an important meeting, an opportunity for all the JRP-Partners to meet each other and to unify the JRP-Consortium around the common set of objectives.

General Project Meetings (GPM) to be attended by representatives of all JRP-Participants will be held once a year, for a period of 1-2 days. Major technical and scientific results and advances will be presented and reviewed, and compared with the planned programme.

o GPM1 around May 14 will be held at BRML

o GPM2 around May 15 will be held at CETIAT

The final meeting will be held at DTI at May 16. It will last two days and will conclude the project.

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Task 5.3: Project reporting (MIKES, all)



A Publishable JRP Summary will be written one month after the signature of the JRP-Contract; this will be updated each half year to reflect the progress of the JRP. (MIKES, all) (D5.3.1)

Interim progress reports will be written after 6, 12, 24 and 30 months. Each WP leader will provide a summary of the status of his workpackage showing the progress of the preceding 6 months against the original schedule and indicate if and where corrective actions might be necessary. The combined progress report of all workpackages will be produced by the JRP-Coordinator. All JRP-Partners and RGs will provide input to the updated JRP Impact report and the JRP-Coordinator will provide this, along with the Interim progress report and an updated Publishable JRP Summary to EURAMET. (MIKES, all) (D5.3.2)

Periodic progress reports will be written after 18 and 36 months. Each WP leader will provide a summary of the status of their workpackage showing the progress of the preceding 6 months against the original schedule. The combined progress report of all workpackages will be produced by the JRP-Coordinator. Full financial reporting and associated audit reports will be supplied by the funded JRP-Partners after 18 and 36 months as required by EURAMET. All JRP-Partners and RGs will provide input to the updated JRP Impact Report. The JRP-Coordinator will provide the Periodic progress report, financial reporting, updated JRP Impact report and updated Publishable JRP Summary to EURAMET. (MIKES, all) (5.3.3)

The Final Publishable Report will be prepared by the JRP-Coordinator at May 16 based on input from all JRP-Partners and RGs, and will contain the final results, conclusions, impact. The JRP-Coordinator will also provide a completed JRP Reporting Questionnaire based on input from all JRP-Partners and RGs. (MIKES, all) (D5.3.4)



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WP5 5.0 0.5 1.5 0.5 0.5 1.5 1.5 0.5 0.5 0.5 1.0 13.5


Deliverable number


Other Participants

Deliverable type

Delivery date

5.3.1 Publishable JRP Summary MIKES All Contract report +30 days after ‘entry into force’ of JRP-Contract

5.3.2 Interim report, updated Publishable JRP Summary, impact report

MIKES All Contract reports

Nov 13, May 14, May 15, Nov 15 (All + 45 days)

EMRP


5.3.3 Periodic report, updated Publishable JRP Summary, impact report, financial audits


Nov 14, May 16 (+ 60 days)

5.3.4 Final publishable report, JRP reporting questionnaire

MIKES All Contract report May 16 (+ 60 days)

EMRP


C6 SUMMARY LIST OF ALL DELIVERABLES

Deliverable number


Other Participants

Deliverable type

Delivery date

1.1.1 Summary report on key findings of literature review

NPL BRML Report Nov 13

1.1.2 LoD primary standard for moisture with sample size smaller than 2 g

NPL Device May 14

1.1.3 Peer-reviewed journal or conference paper on validating NPL’s primary standard for moisture submitted

NPL Publication Nov 14

1.1.4 LoD primary standard for moisture with sample size up to 200 g

DTI Device May 14

1.1.5 Peer-reviewed journal or conference paper on validating DTI’s primary standard for moisture submitted

DTI Publication Nov 14

1.1.6 Peer-reviewed journal or conference paper publishing the MIKES research system submitted

MIKES Publication Nov 14

1.1.7 Comparison data between the SI traceable moisture realisations and relevant standardised moisture determinations for selected materials in pharmaceuticals, foodstuff, feed, biomass, wood and paper

MIKES BRML, DTI, NPL, TUBITAK

Data set May 15

1.1.8 Peer-reviewed journal or conference paper on uncertainty estimation tools for gravimetric SI moisture unit realisation submitted

TUBITAK BRML, DTI, MIKES, NPL

Publication Mar 16

1.2.1 Literature survey of the factors determining the uncertainty of cKF method and their contributions

UT Report Sep 13

1.2.2 Coulometric KF measurement setups and the initial method set up at JRP-Partners' labs

UT BRML Device Mar 14

1.2.3 Report on the interaction between sample and its environment during the cKF analysis and a validated procedure to minimise the corresponding uncertainty

BRML UT Report Sep 14

1.2.4 Final cKF method including the sample handling part is available and validated

UT BRML Procedure Jan 15

1.2.5 Validation report and uncertainty budget available for the coulometric KF method

UT BRML Report Jul 15

1.3.1 Report on the review of terms and definitions in moisture measurements

NPL Report May 15

1.3.2 Report on the comparison of the cKF results with LoD method for polymer samples

UT BRML, TUBITAK

Report Nov 15

EMRP


1.3.3 Report on the comparison with foodstuff and biomass relevant samples with two different moisture content levels measured using the LoD methods

MIKES BRML, CETIAT, DTI, NPL, TUBITAK

Report Jan 16

1.3.4 Report on the comparison of the developed primary standards using new CRMs developed in WP2

NPL DTI, TUBITAK, BRML

Report Feb 16

1.3.5 Draft document recommending terms, definitions, realisations and principles of SI traceability for moisture measurements

MIKES DTI, CETIAT, NPL, UT, TUBITAK

Discussion draft

Jan 14

1.3.6 Paper on comparisons and traceability for moisture measurements submitted to a peer-reviewed journal

MIKES DTI, CETIAT, NPL, UT, TUBITAK

Publication Mar 16

2.1.1 The list of candidate materials prepared

NPL BRML, UT Report May 14

2.1.2 Uncertainty analysis data for CRM NPL BRML, UT Data Jan 15

2.1.3 At least one new CRM available NPL BRML, UT Artefact Sep 15

2.2.1 Review report on procedures relevant to transportation of samples and CRMs

BRML Report May 14

2.2.2 Submission of peer-reviewed journal or conference paper on the RH/T logger based sample monitoring method to quantify the effect of transportation on the stability of processed wood and biomass samples

MIKES Publication Jul 15

2.2.3 Submission of peer-reviewed journal or conference paper on the effect of ambient conditions and packaging on the stability of wooden samples during transportation

CMI MIKES Publication Mar 15

2.2.4 At least 3 sample holders designed and tested

INRIM Artefact Sep 14

2.2.5 Submission of peer-reviewed journal or conference paper on the effect of ambient conditions and packaging on the stability of food and pharmaceutical powders and paper samples during transportation

BRML TUBITAK Publication Nov 14

2.2.6 Report on potentiality of applying a correction factor to reduce the effect of transportation

MIKES CMI Report Aug 15

2.2.7 Good practice guide for estimating the uncertainty due to sample handling and transportation

CMI BRML, MIKES, TUBITAK

Good Practice Guide

Sep 15

2.3.1 Design of resonant or non resonant coaxial cells for RF/MW transfer standard instrument

CETIAT Design May 14

2.3.2 At least 4 resonant or non resonant coaxial cells ready

CETIAT Device Nov 14

2.3.3 Complete RF/MW transfer system with initial tests

CETIAT Device Mar 15

EMRP


2.3.4 Conference report or publication on the transfer standard using microwaves and radio frequencies approach and its validation

CETIAT Publication Sep 15

2.3.5 Microwave moisture meter INRIM Device Nov 14

2.3.6 Portable humidity generator INRIM Device Mar 14

2.3.7 Complete transfer standard system with initial tests

INRIM Device Sep 15

2.3.8 Conference report or publication on transfer standard system comprising MW moisture meter and a portable humidity generator

INRIM Publication Jan 16

2.3.9 Reference measurements for transfer standards tests

TUBITAK Dataset Jan 16

2.4.1 Design of a calibration system for sensors measuring surface moisture in polymer elements

UL Design May 14

2.4.2 Complete system with initial tests UL Device May 15

2.4.3 Design of a calibration system for sensors measuring surface moisture in plastic/paper elements

TUBITAK Design May 14

2.4.4 Complete system with initial tests TUBITAK Device May 15

2.4.5 Report on validation of calibration methods for surface moisture meters including uncertainty evaluations

UL TUBITAK, CMI Report May 16

3.1.1 (REG D1.2)

Mathematical modelling of moisture processes in selected materials

INRIM REG (UNICLAM)

Report Feb 14

3.1.2 Model of temperature distribution CMI Report Aug 14

3.1.3

(REG D1.3)

Numerical model and code to investigate time-dependent moisture and thermal profile in selected materials

REG (UNICLAM)

Software tool May 14

3.1.4 Submission of peer-reviewed Journal or conference paper on mathematical modelling of moisture processes

INRIM TUBITAK, REG (UNICLAM)

Publication Nov 14

3.1.5 Report on modelling of mass transfer in drying of selected materials and how this affects an inline moisture sensor

DTI Report Nov 14

3.1.6 Model for diffusion of moisture in paper sheet

TUBITAK Model Nov 14

3.1.7 Report on model verification REG (UNICLAM)

DTI Report May 15

3.2.1 (REG D3.1)

Report on design of experiments for modelling validation


Report Jul 15

3.2.2 (REG D3.2)

Report on validation of numerical tools for moisture models


Report Sep 15

3.2.3 Report on validation of the calibration method for surface moisture

UL Report Nov 15

3.2.4 Report on validation of microwave measurement method for bulk moisture

INRIM Report Aug 15

EMRP


3.2.5 Journal or conference paper on interaction between the measurand and the measuring instrumentation in moisture metrology submitted

INRIM CMI, UL Publication Nov 15

3.2.6 Report on impact of thermal effects and local temperature distribution on moisture content measurements

CMI Report Aug 15

3.2.7 (REG D3.4)

Report on the application of the modelling software tool

REG (UNICLAM)

DTI, TUBITAK Report May 16

3.3.1 (REG D3.3)

Report on uncertainty analysis of numerical modelling

INRIM REG (UNICLAM)

Report Mar 16

3.3.2 Report on uncertainty evaluations for moisture measurements in paper

TUBITAK BRML Report Mar 16

3.3.3 Model uncertainty budgets based on spreadsheet form targeted to calibration and testing laboratories

INRIM BRML, TUBITAK, UT

Software tool Mar 16

4.1.1 Liaison with stakeholders though two-way sharing of information, by correspondence, meetings and visits

MIKES All Reports May 14, May 15, May 16

4.1.2 Registration, design, and maintenance of website with content management allowing inputs of JRP-Partners, updated every 6 months

UL All JRP web site Aug 13, Nov 13, May 14, Nov 14, May 15, Nov 15, May 16

4.1.3 Active input and dissemination though sector technical and standards committees

NPL INRIM

DTI

Reports May 14, May 15, May 16

4.1.4 At least 5 presentations at conferences, presenting overview or individual outputs of the project

MIKES BRML, CETIAT, DTI, NPL, REG (UNICLAM)

Conference presentations

May 14, Nov 14, Sep 15, Nov 15

4.1.5 At least 5 paper or electronic publications spanning trade magazines, sector-specific and measurement journals

DTI

BRML, CETIAT

Publications May 14, May 15, Apr 16

4.1.6 Guide on Karl-Fischer titration usage and uncertainty evaluation

UT DTI Good practice guide

Sep 15

4.2.1 Develop new training course material and case studies

CETIAT DTI, UT Progress report

Training course material

Nov 14

Apr 16

4.2.2 Workshops including scientific reports of the project and/or training elements

CETIAT INRIM, MIKES, TUBITAK, REG (UNICLAM)

Workshops Nov 14, May 15, Nov 15, May 16

4.2.3

(REG D4.6)

2-way training during Guestworking REG

(UNICLAM)

DTI Training Apr 15

4.3.1 Two-way liaison with relevant groups in IMEKO, EURAMET and other RMOs, and relevant CIPM CCs

NPL DTI, MIKES Reports May 14, May 15, May 16

EMRP


4.3.2 Report proposing future actions on international metrological infrastructure for moisture metrology

NPL All Report Mar 16

4.4.1 New/improved calibration, sampling and measurement services

BRML DTI, MIKES, NPL, TUBITAK

Progress report

Service

Nov 14

Mar 16

4.4.2 Extend upon existing consulting services

INRIM DTI, MIKES Consultancy service

May 15

4.4.3 Report on the exploitation route for new CRM(s) developed during the project

NPL BRML, UT Report Apr 16

5.3.1 Publishable JRP Summary MIKES All Contract report +30 days after ‘entry into force’ of JRP-Contract

5.3.2 Interim report, updated Publishable JRP Summary, impact report


Nov 13, May 14, May 15, Nov 15 (All + 45 days)

5.3.3 Periodic report, updated Publishable JRP Summary, impact report, financial audits


Nov 14, May 16 (+ 60 days)

5.3.4 Final publishable report, JRP reporting questionnaire

MIKES All Contract report May 16 (+ 60 days)

EMRP


C7 THE PROJECT TIMESCALE: GANTT CHART

C7.a GANTT chart for WP1

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Task 1.1 Development of gravimetric realisation methods (leader:MIKES)

D1.1.1 Summary report on key f indings of literature review

(NPL, BRML)D

D1.1.2 LoD primary standard for moisture w ith sample size smaller than

2 g (NPL)D

D1.1.3 Peer-review ed Journal or conference paper on validating NPL's

primary standard for moisture submitted (NPL)D

D1.1.4 LoD primary standard for moisture w ith sample size up to 200 g

(DTI)D

D1.1.5 Peer review ed journal or conference paper on validating DTI's

primary standard for moisture submitted (DTI)D

D1.1.6 Peer review ed journal or conference paper publishing the MIKES

research system submitted (MIKES)D

D1.1.7 Comparison data betw een the SI traceable moisture realisations

and relevant standardised moisture determinations (MIKES,

BRML, CMI, NPL, TUBITAK)

D

D1.1.8 Peer-review ed Journal or conference paper on uncertainty

estimation tools for gravimetric SI moisture unit realisation

submitted (TUBITAK, BRML, DTI, MIKES, NPL)

D

Task 1.2 Improved Karl Fischer titration realisation methods (leader: UT)

D1.2.1 Literature survey of the factors determining the uncertainty of

coulometric KF titration and their contributions (UT)D

D1.2.2 Coulometric KF measurement setups and the initial method set

up at JRP-Partners' labs (UT, BRML)D

D1.2.3 Report on the interaction betw een sample and its environment

during the cKF analysis and a validated procedure to minimise

the corresponding uncertainty (BRML, UT)

D

D1.2.4 Final cKF method including the sample handling part is available

and validated (UT, BRML)D

D1.2.5 Validation report and uncertainty budget available for the

coulometric KF method (UT, BRML)D

Task 1.3 Principles of SI traceability (leader:MIKES)

D1.3.1 Report on the review of terms and definitions in moisture

measurements (NPL)D

D1.3.2 Report on the comparison of the cKF results w ith LoD method

for polymer samples (UT, BRML, TUBITAK)D

D1.3.3 Report on the comparison w ith foodstuff and biomass relevant

samples using the LoD methods (MIKES, BRML, CETIAT, DTI,

NPL, TUBITAK)

D

D1.3.4 Report on the comparison of the developed primary standards

using new CRMs developed in WP2 (NPL, BRML, DTI, TUBITAK) D

D1.3.5 Draft document recommending terms, definitions, realisations

and principles of SI traceability for moisture measurements

(MIKES, DTI, CETIAT, NPL, TUBITAK, UT)

D

D1.3.6 Paper on comparisons and traceability for moisture

measurements submitted to peer-review ed journal (MIKES, CMI,

DTI, CETIAT, NPL, TUBITAK, UT)

D

EMRP


C7.b GANTT chart for WP2

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Task 2.1 New CRMs (leader:NPL)

D2.1.1 The list of candidate materials prepared (NPL, BRML, UT) DD2.1.2 Uncertainty analysis dat for CRM (NPL, BRML, UT) DD2.1.3 At least one new CRM available (NPL, BRML, UT) D

Task 2.2 Improved methods for handling and transporting samples (leader: MIKES)

D2.2.1 Review report on procedures relevant to transportation of

samples and CRMs (BRML)D

D2.2.2 Submission of peer-review ed Journal or conference paper on

the RH/T logger based sample monitoring method... (MIKES)D


the effect of ambient conditions and packaging on the stability of

w ooden samples during transportation (CMI, MIKES)

D

D2.2.4 At least 3 sample holders designed and tested (INRIM) DD2.2.5 Submission of journal or conference paper on the effect of

ambient conditions and packaging on the stability... (BRML,

TUBITAK)

D

D2.2.6 Report on potetiality of applying a correction factor to reduce the

effect of transportation (MIKES, CMI)D

D2.2.7 Good practice guide for estimating the uncertainty due to sample

handling and transp. (CMI, BRML, MIKES, TUBITAK)D

Task 2.3 New transfer standards (leader: CETIAT)

D2.3.1 Design of resonant of non resonant coaxial cells for RF/MW

transfer standard instrument (CETIAT)D

D2.3.2 At least 4 resonant or non resonant coaxial cells ready

(CETIAT)D

D2.3.3 Complete RF/MW transfer system w ith initial tests (CETIAT) DD2.3.4 Conference report or publication on the transfer standard using

microw aves and radio frequencies...(CETIAT)D

D2.3.5 Microw ave moisture meter (INRIM) DD2.3.6 Portable humidity generator (INRIM) DD2.3.7 Complete transfer standard system w ith initial tests (INRIM) DD2.3.8 Conference report or publication on transfer standard system

comprising MW moisture meter and a portable humidity generator

(INRIM)

D

D2.3.9 Reference measurements for transfer standards tests

(TUBITAK)

Task 2.4 Novel calibration methods for surface moisture meters (leader: UL)

D2.4.1 Design of calibration system for sensors measuring surface

moisture in polymer elements (UL)D

D2.4.2 Complete system w ith initial tests (UL) DD2.4.3 Design of calibration system for sensors measuring surface

moisture in plastic/paper elements (TUBITAK)D

D2.4.4 Complete system w ith initial tests (TUBITAK) DD2.4.5 Report on validation of calibration methods for surface moisture

meters including uncertainty evaluations (UL, TUBITAK, CMI) D

EMRP


C7.c GANTT chart for WP3

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Task 3.1 Modelling (leader:INRIM)

D3.1.1 Mathematical modelling of moisture processes in selected

materials (INRIM, REG(UNICLAM))D

D3.1.2 Model of temperature distribution (CMI) DD3.1.3 Numerical model and code to investigate time-dependent

moisture and thermal profile in selected materials

(REG(UNICLAM))

D


mathematical modelling of moisture processes (INRIM, TUBITAK,

REG(UNICLAM))

D

D3.1.5 Report on modeling of mass transfer in drying of selected

materials and how this affects an inline moisture sensor (DTI)D

D3.1.6 Model for diffusion of moisture in paper sheet (TUBITAK) DD3.1.7 Report on model verif ication (REG(UNICLAM)) D

Task 3.2 Selected experimental validation of models (leader: CMI)

D3.2.1 Report on design of experiments for modelling validation (INRIM,

UL, REG(UNICLAM))D

D3.2.2 Report on validation of numerical tools for moisture models

(INRIM, REG(UNICLAM))D

D3.2.3 Report on validation w ith the sensor calibration method for

surface moisture (UL)D

D3.2.4 Report on validation of microw ave measurement method for bulk

moisture (INRIM)D

D3.2.5 Journal or conference paper on interaction betw een the

measurand and the measuring instrumentation in moisture

metrology submitted (INRIM, CMI, UL)

D

D3.2.6 Report on impact of thermal effects and local temperature

distribution on moisture content measurements (CMI)D

D3.2.7 Report on the application of the modelling softw are tool

(REG(UNICLAM), DTI, TUBITAK)D

Task 3.3 Model uncertainty analysis (leader: TUBITAK)

D3.3.1 Report on uncertainty analysis of numerical modelling (INRIM,

UNICLAM)D

D3.3.2 Report on uncertainty evaluations for moisture measurements in

paper (TUBITAK, BRML)D

D3.3.3 Model uncertainty budgets based on spreadsheet form targeted

to calibration and testing laboratories (INRIM, BRML, TUBITAK

UT)

D

EMRP


C7.d GANTT chart for WP4

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Task 4.1 Knowledge transfer (leader:MIKES)

D4.1.1 Liaison w ith stakeholders though tw o-w ay sharing of

information, by correspondence, meetings and visits (MIKES,

all)

X X D

D4.1.2 Registration, design, and maintenance of w ebsite w ith content

management allow ing inputs of JRP partners. Updated every 6

months (UL, all)

X X X X X X D

D4.1.3 Active input and dissemination through sector technical and

standards committees (NPL, INRIM, CETIAT)X X D

D4.1.4 At least 5 presentations at conferences, presenting overview or

individual outputs of the project (BRML, CETIAT, DTI, MIKES,

NPL, REG(UNICLAM))

X X X D

D4.1.5 At least 5 paper or electronic publications spanning trade

magazines, sector-specif ic and measurement journals (DTI,

BRML, CETIAT)

X X D

D4.1.6 Guide on Karl-Fischer titration usage and uncertainty evaluation

(UT, DTI)D

Task 4.2 Training (leader: CETIAT)

D4.2.1 Develop new training course material and case studies

(CETIAT, DTI, UT)X D

D4.2.2 Workshops including scientif ic reports of the project and/or

training elements (CETIAT, INRIM, MIKES, TUBITAK, UNICLAM) X X X D

Task 4.3 Metrology infrastructure building (leader: NPL)

D4.3.1 Tw o-w ay liaison w ith relevant groups in IMEKO, EURAMET and

other RMOs, and relevant CIPM CCs (NPL, All)X X D

D4.3.2 Report proposing future actions on international metrological

infrastructure for moisture metrology (NPL, All)D

Task 4.4 Exploitation (leader: NPL)

D4.4.1 New /Improved calibration, sampling and measurement services

(BRML, DTI, MIKES, NPL, TUBITAK)X D

D4.4.2 Extend upon existing consulting services (INRIM, DTI, MIKES) DD4.4.3 Report on the exploitation route for new CRM(s) developed

during the project (NPL, BRML, UT)D

EMRP


C7.e GANTT chart for WP5

EMRP


Section D: Risk and Risk Mitigation

D1 SCIENTIFIC/TECHNICAL RISKS

Risk (description) Likelihood and impact of occurrence

Mitigation Contingency

WP1, Task 1.1 The uncertainty of a primary standard is higher than expected or a primary standard has a systematic error that is not taken into account

Likelihood without mitigation: Medium Impact: Faulty uncertainty statements might be used; the intercomparison would be less conclusive Likelihood after mitigation: Low

Comparing different principles, i.e. cKF and LoD primary standards, and having more than one lab building the same type but via different technical approaches reduces the chance of not finding systematic errors or outliers

Perform an outlier test in the comparison and find the new mean value and En values

WP1, Task 1.1 Risk that aspects of the performance of a commercial instrument cannot practically be tested and validated

Likelihood without mitigation: Medium Impact: Only DTI would have a primary standard for water mass fraction Likelihood after mitigation: Low

Maintain a good relationship with the instrument supplier, who will support non-routine work with the instrument

In the case of a serious obstacle to primary validation, useful knowledge will still be gained and disseminated Future adaptations could be proposed Establishing traceability to the DTI primary standard

WP1, Task 1.2 Impossible to achieve as low an uncertainty as planned with the cKF method

Likelihood without mitigation: Medium Impact: Uncertainty better than the state of the art would not be achieved Likelihood after mitigation: Low

Two laboratories work on this task using three different coulometric KF titrator models and two different sample preparation systems; it would be sufficient if just one lab with one experimental setup achieved the necessary uncertainty

Better uncertainty could be achieved by using two different systems together (i.e. using multiple analyses with different methods)

WP1, Task 1.3 The quality of the comparison results is not good enough for serving as a basis for the recommendation on the principles of SI traceability due to problems with sample handling

Likelihood without mitigation: High Impact: Useful recommendation could not be prepared Likelihood after mitigation: Low

Efforts to reduce the effect of sample handling in Task 2.2 (WP2) and addressing specifically this issue in the primary standard development Cooperation with collaborators with strong experience in sample handling

Additional comparison measurements combined with interlaboratory training on the sample handling among the JRP-Partners

WP2, Task 2.1 No useful new CRM can be identified or characterised

Likelihood without mitigation: Medium Impact: The project would not deliver new CRMs and would fail to improve this aspect of traceability provision Likelihood after mitigation: Low

Input from collaborator LGC, who have extensive expertise in CRMs Multiple measurement techniques, improved within the project

Materials may provide useful checks or studies, if not CRMs; useful knowledge will still be gained and disseminated Possibilities to engage LGC and other relevant collaborators in a joint project beyond this project will be explored Potential introduction of a Stage 3 REG and/or RMG

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WP2, Task 2.3 The RF/MW transfer standard to be developed is too sensitive to variations in samples and sample conditions

Likelihood without mitigation: Medium Impact: The uncertainty level required in the dissemination of SI traceability is not achieved with the RF/MW Likelihood after mitigation: Low

Collaboration between several JRP-Partners having solid experience on microwave techniques Two different approaches to develop transfer standard instruments

In a case that the RF/MW instrument does not fulfil the requirements, there is the other type of transfer standard available Possibly combining the two types of transfer standards

WP2, Task 2.4 Model for surface moisture measurement cannot be validated with TGA

Likelihood without mitigation: Medium Impact: Calibration uncertainty for surface moisture meters cannot be determined Likelihood after mitigation: Low

Experience gained in WP1 and Task 2.2 will be exploited through close collaboration between the JRP-Partners

Other moisture analysis available at the JRP-Partner institutes will be exploited

WP3, Task 3.1 Computation time too high to achieve the required accuracy for all cases

Likelihood without mitigation: Medium Impact: Some cases cannot be computed or need to be computed with lower accuracy Likelihood after mitigation: Low

Increase the computational capacity

Limit the cases by identifying the most important and usable ones and perform the computation primarily for them

WP4 Risk that committee cooperation at CC, RMO, and other levels does not achieve progress on CMCs, kcs and other harmonisation in the field

Likelihood without mitigation: Medium to high Impact: Very limited progress in the international recognition of national moisture standards Likelihood after mitigation: Low to medium

A recognised, funded JRP, with clear objectives on this, will greatly strengthen prospects of active cooperation and joint working among relevant groups Active cooperation through many already established channels of contacts

If the JRP achieves limited progress in enhancing the international harmonisation, it will nonetheless lay foundations for future progress after the lifetime of the JRP; a report will make recommendations for future work and the established network of relevant key people will be used for finding a roadmap to the aimed level

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D2 MANAGEMENT RISKS

Risk (description) Likelihood and impact of occurrence

Mitigation Contingency

Key personnel are lost to the project

Likelihood without mitigation: Medium (none of the named key persons is planning to leave the project within its duration) Impact: Valuable experience and input is lost with a leaving person; delays Likelihood after mitigation: Low

The JRP brings together a large number of experts from many institutes and within them; open, visible and close collaboration within the JRP-Consortium ensures effective exchange of knowledge reducing the impact of the loss of a single person All key personnel have experienced deputies who will be well informed about the progress of the project

Delays will be coped with by re-scheduling work As an extreme option, work can be re-allocated between JRP-Partners

Deliverables are not delivered according to the schedule

Likelihood without mitigation: High Impact: Further delays are caused because of the interrelation between tasks and WPs Likelihood after mitigation: Low

Regular communication between the WP leaders (the Project Management Board) and between all JRP-Partners via e-mails and scheduled meetings; all WP leaders can also host ad-hoc internet meetings whenever problems appear In the kick-off, May 14 and May 15 meetings, the content and schedule of all deliverables will be clarified

If the delays jeopardise the Task or WP, the Project Management Board will meet and agree actions to prevent failure, mainly by re-allocating the work

IPR – Intellectual Property Rights: Exploitation of the scientific outcomes could be a source of potential conflicts between JRP-Partners

Likelihood without mitigation: Medium Impact: Conflicts delay progress in the JRP Likelihood after mitigation: Low

IP agreement will be made at JRP-Contract stage to prevent the conflicts and to help the Project Management Board to efficiently solve any confusion or disagreement between JRP-Partners IP issues will also be checked in all project meetings

If a disagreement comes up and it cannot be solved by the PMB, an independent arbitrator will be used

REG-Researcher decides not to accept the grant or leaves before the end of REG duration

Likelihood without mitigation: Medium Impact: The tasks assigned to REG will not be carried out in full Likelihood after mitigation: Low

REG Home Organisation identifies potential replacement researcher Potentiality to apply stage 3 REG will be explored

Some parts of the REG work can be merged with the tasks of the JRP-Partners enabling progress critical for successful completion of other task

Work load of the JRP-Coordinator is too large preventing efficient project management

Likelihood without mitigation: Medium Impact: Delays in reporting and increased risks of the cumulating technical problems Likelihood after mitigation: Very low

MIKES will reserve a sufficient portion of the JRP-Coordinator’s working hours for the JRP management and provides sufficient financial and secretarial support

As a final resort, MIKES will assign a vice-coordinator for the project to reduce the workload of the JRP-Coordinator

D3 ETHICAL ISSUES

The research in this JRP does not incorporate any risks of conflict with ethical norms.

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Section E: Project Resources and Budget Overview

E1 JRP LABOUR RESOURCES (Person Months) 1-

MIK

ES

2- B

RM

L

3- C

ETIA

T4-

CM

I

5- D

TI

6- IN

RIM

7- N

PL

8- T

UBIT

AK

9- U

L

10- U

T

11- R

EG

(UN

ICLA

M)

TO

TA

L

WP1 14.0 18.0 2.5 13.0 14.5 7.0 28.5 97.5

WP2 7.0 9.5 13.0 10.0 11.0 12.5 7.0 11.6 2.0 83.6

WP3 10.0 7.0 1.0 17.0 6.0 3.5 2.0 33.0 79.5

WP4 2.0 2.0 2.0 2.0 1.8 2.0 4.0 1.7 1.5 3.0 2.0 24.0

WP5 5.0 0.5 1.5 0.5 0.5 1.5 1.5 0.5 0.5 0.5 1.0 13.5

TOTAL 28.0 40.0 19.0 19.5 16.3 31.5 32.5 22.2 17.1 36.0 36.0 298.1

E2 JRP BUDGET BREAKDOWN

Labour (€) 1 190 756.31

T&S (€) 64 190.78

Equipment (€ 36 184.89

Consumables (€) 70 140.50

Other costs (€) 29 550.00

Sub-contracting (€) 30 910.67

Third Party resources (€)

Overhead (€) 1 295 296.96

Total eligible costs (€) 2 717 030.11

EURAMET contribution (€) 1 162 888.89

E3 RATIONALE FOR NON-LABOUR RESOURCES

T&S (Travel and Subsistence):

MIKES 6 000 4 project meetings; stakeholder activity; travel to other JRP-Partners

BRML 5 000 4 project meetings; 2 conferences

CETIAT 8 500 4 project meetings; 2 conferences

CMI 5 800 4 project meetings; 3 workshops

DTI 5 250 4 project meetings; visit stakeholders; 1 conference

INRIM 7 400 4 project meetings; dissemination activity; travel to other JRP-Partners

NPL 5 241 4 project meetings; workshops; conferences; local travel to UK stakeholders

TUBITAK 10 800 4 project meetings x 2 people; 2 conferences x 2 people; training visit x 2 people

UL 7 200 4 project meetings; workshops; conferences

UT 3 000 4 project meetings

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Equipment

It is planned to purchase the following equipment:

- 17 185 € for equipment for the NPL primary moisture standard

- 19 000 € for coulometric KF titrator with a sample oven at UT

Consumables

70 140.50 € has been included for consumables including

- mechanical components - CRMs - glassware - vacuum components - electrical components - chemicals - samples for measurements - nitrogen gas - distilled water - bath alcohol - electronic parts

Other costs

29 550.00 € has been included for other costs including

- catering for project meetings - conference fees - chemical analysis - stainless steel welding and assembly - electronic parts

Sub-contracting

30 910.67 € has been included for sub-contracting consisting of financial audit costs.

Third party

None to be charged to the JRP.

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Section F: Rationale for the JRP-Consortium

The named individuals give an indication of the experts who will deliver the JRP, however the JRP-Protocol will not be updated if personnel change (except in the case of the JRP-Coordinator).

F1 DESCRIPTION OF EACH JRP-PARTICIPANT (EXCEPT COLLABORATORS), INCLUDING KEY ROLES AND CONTRIBUTIONS

JRP-Participant 1 - MIKES (JRP-Coordinator, funded JRP-Partner)

As the National Metrology Institute of Finland, the Centre for Metrology and Accreditation (MIKES) realises the SI units, performs high-level metrological research and develops measuring applications in partnership with industry. The MIKES calibration and expert service is vital for Finnish industry in reaching success in global markets with minimum environmental impact and for society in ensuring safety and welfare.

In this JRP, MIKES will exploit its extensive experience in research, development and calibration services in the fields of humidity and moisture, temperature, gas flow and mass measurements. MIKES has developed many facilities for research, calibration and testing in industry, at MIKES and in other national metrology institutes. In the field of moisture in solids, MIKES has studied the reliability of moisture measurements in paper and foodstuff in specific applications. Other recent research topics at MIKES relevant to this JRP include the development of various types of humidity generators, an air speed determination method based on water vapour as a trace gas, a calibration method for nanoforce sensors and syringe pumps, a study on dynamic calibration for RH/T meters and loggers, comparison methods for humidity standards, and a study on heat and mass transfer in a measurements chamber using numerical simulation.

In WP1, MIKES will study the effect of water binding and volatiles on moisture measurements in biomass and wooden material samples with a novel research system developed in this project. MIKES will also contribute to the analysis of the WP1 results, interlaboratory comparisons and formulation of principles for SI traceability. MIKES will also use the research system in WP2 combined with NIR, IR and/or NMR instruments for studying error sources in transportation of processed wood and biomass samples. The experience from RH/T instruments and loggers will be used in developing a new method for quantifying the transportation effect on the basis of conditions monitoring. MIKES will exploit its close collaboration with Finnish industrial companies identified as collaborators of this JRP.

As the JRP-Coordinator, Martti Heinonen of MIKES, has excellent project management skills, having led and currently leading a number of multi-national projects in the framework of EUROMET/EURAMET. He was a WP leader in the iMERA Plus JRP T3.J1.1 Nanoparticles and is currently leading a WP in the EMRP JRP ENG01 GAS.

Key scientific personnel:

Adj. prof. Martti Heinonen, head of the Thermal and Mass Quantities Group at MIKES, will lead WP1. As the JRP-Coordinator, he also will lead WP5 (Management). He has been carrying out research on humidity and moisture related metrology for over 20 years resulting in over 80 published papers. He chaired the EURAMET TC-T Humidity subcommittee from 2004 to 2008 and currently chairs the EURAMET TC-T Best Practice Group. He represents MIKES in CCT (incl. WG6 Humidity and WG Strategy), EURAMET TC-T (incl. Strategy Group and CMC Review Group) and EURAMET TC-F. He is a member of NCSLI and IMEKO TC12 and a scientific supervisor in JRP ENV07 MeteoMet. He was a member of the Scientific committee of the 7th Int. Conference on Water in Food. He has been supervising several doctoral theses in relevant metrology fields.

Dr Kari Riski, head of the mass laboratory at MIKES, has worked on mass metrology for over 25 years and authored over 80 published papers. He represents MIKES in EURAMET TC-M. He is also experienced in research on thermometry. In this project he will contribute to the developments related to gravimetric measurements.

Key publications:

M. Heinonen et al., Investigation of the equivalence of national dew-point temperature realisations in the range -50 °C to +20 °C, Int. J. Thermophys., 10.1007/s10765-011-0950-x

S. Sillanpää, M. Heinonen, A mixing method for traceable air velocity measurements, Meas. Sci. Technol. 19 (2008) 085409M

S. Saxholm, M. Heinonen, A calibration system for PTU devices, Measurement 43 (2010) 1583–1588

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L. Stenlund, K. Riski, J. Seppä; M. Pudas, M. Vähäsöyrinki, V. Tuhkanen and J. Röning, Traceable characterisation of a bending millimetre scale cantilever for Nanoforce sensing, Meas. Sci. Technol., 21 (2010) 075102

JRP-Participant 2 - BRML (funded JRP-Partner)

The National Institute of Metrology (BRML) is a research and development institute under the Romanian Bureau of Legal Metrology (Biroul Roman de Metrologie Legala, BRML), actively involved in research projects aiming at developing, characterising and improving different measurement standards and instruments as well as measurement methods used in different fields of metrology for more than 15 years. Due to the economic impact, a lot of activities have been performed to develop measurement standards and methods related to moisture in solids, gases and liquids. BRML has nominated this project as the key strategic priority for Romania.

Within the Reference Materials Group, moisture in solids is measured using gravimetric methods and it is applied to a wide range of matrixes such as grains, oilseeds, wood, paper, etc. The reference measurements standard includes a Mettler Toledo LJ 16 Moisture Analyser and ovens with and without air convection. The same group has developed electrochemical Karl-Fischer measurements – both potentiometry and coulometry. Several studies aimed at developing working standards for water in oil products, measurements procedures and putting into evidence different sources of uncertainty. Mainly the Karl Fisher coulometer Cou-Lo Compact and a Schott Titroline Plus titrator were used in such research activities.

BRML will contribute to the development of new methods and measurements standards in WP1, and to modelling measurement processes and identifying main uncertainty components in WP3.


Dr Mirella Buzoianu is experienced in Reference Materials and contributed to the development of the Karl-Fischer method in the BRML.

Senior researcher Ileana Nicolescu is an experienced senior researcher participating in more than 20 research projects within the national research programs. Her experience in analytical chemistry, of experiments using a wide range of analytical methods, brings to this project proven expertise for WP1.

Dr Ionescu George Victor has extensive experience in calibrating and testing humidity meters for moisture in grains and oilseeds.

Key publications:

Ionescu G. V, Buzoianu M. Popescu I.M., “Uncertainty evaluation of the Romanian reference standard for cereals moisture”, OIML Bulletin, 2004, vol. XLV, No. 2: 5-9

Mirella Buzoianu. “New developments in the production and use of CRMs”, AQUAL, 2003, No. 8: 124-129

JRP-Participant 3 - CETIAT (funded JRP-Partner)

CETIAT (Centre Technique des Industrie Aéraulique et Thermique) is a study, testing and calibration laboratory in the fields of aerodynamics and fluid mechanics, heat sciences, and acoustics. CETIAT provides a tailor-made service for industrials wishing to benefit from the competencies and technical means developed since the creation of CETIAT in 1960. CETIAT has been granted the status of Industrial Technical Centre, which enables it to allocate each year a budget of 2.5 million € to the performance of a collaborative studies programme for its 275 industrial affiliates. There is a staff of 120, among which 80 people are engineers and technicians. CETIAT is an associated laboratory of the LNE (Laboratoire National de Métrologie et d’Essais). CETIAT is in charge of research and traceability for three units in the French metrological chain. The researcher involved in this JRP works in a sub field of thermometry: hygrometry. The hygrometry laboratory in the CETIAT is in charge of the realisation of the national humidity standards at the highest level of accuracy.

CETIAT will lead WP2 and develop a new RF/MW transfer standard. CETIAT will also contribute to comparison measurements in WP1.


Dr Eric Georgin has been responsible for the humidity laboratory at the Metrological Department of CETIAT for 4 years. He is responsible for humidity calibration activity, metrological studies in the field of humidity measurement and is the French contact person for the sub-field humidity of the EURAMET Technical Committee in Thermometry. He has experience in uncertainty analysis and he is involved in EURAMET and

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EMRP projects including EURAMET 1034 “Determination of the water vapor pressure curve, between -100 °C and 100 °C, with a very high accuracy” and EMRP JRP-ENV07 MeteoMet.

Jean François Rochas has been working at CETIAT as a project manager since 2007. He has 36 years of experience in the field of high frequencies and micro-waves applications dedicated to industrial process.

Key publications

S. Mokdad, E. Georgin, Y. Hermier, F. Sparasci, M. Himbert, Development of a quasi-adiabatic calorimeter for the determination of the water vapour pressure curve, Rev Sci Instrum. 2012 Jul;83(7):075114

S. Mokdad, E. Georgin, I. Mokbel, J. Jose, Y. Hermier, M. Himbert, On the Way of Determination of the Vapour-Pressure Curve of Pure Water, International Journal of Thermophysics, 2012

G. Roussy, J-F. Rochas, D. Vuillot and C. Debard,” A critical look at permittivity and permeability measurement methods in waveguide. An elementary data fusion approach”, JMPEE, Volume 43, Number 4, pp. 28-36, 2010

JRP-Participant 4 - CMI (funded JRP-Partner)

The Czech metrology institute (CMI) is the national metrology institute of the Czech Republic. CMI is the custodian of the Czech national standards. Its purpose is to realise and maintain the standards of physical units, to provide calibration and verification of measurement instruments for customers and to undertake research and development connected to standards and measurement techniques. CMI fulfils the tasks concerning the membership of the Czech Republic in the relevant international metrological organisations (BIPM, CIPM, OIML, EURAMET). CMI is notified body No. 1383 (Authorised body No. 250).

The laboratory of moisture solids is the one part of the regional branch of the Czech metrology institute in Pardubice. This laboratory specialises in moisture in grain, oilseeds and wood (laboratory is under accreditation), but the laboratory also performs moisture measurements in papers, textiles and plastic samples. This laboratory has gravimetric facilities, which includes two drying machines, two weighing machines and many exsiccators with desiccant. The laboratory is able to measure gravimetrically the moisture of grains and oilseeds from 4 % to 50 % relative moisture and the moisture of wood, textiles and papers from 4 % to 100 % relative moisture. This laboratory has facilities for volumetric Karl-Fischer titration. The laboratory can measure moisture of plastic samples and many other materials (solid and liquid) from 100 ppm to 100 %.

The Thermal Properties Department of CMI will also participate in this JRP. It carries out research and provides measurement services in temperature and humidity metrology. Research activities in the humidity area are focused on the development and improvement of a primary humidity generator for air at atmospheric pressure and for other gases at pressures up to 15 MPa. Research activities in the thermometry area include surface temperature measurements and modelling of potential in solid materials.

CMI will contribute to the research on handling and transportation of samples as well as calibration methods for surface moisture meters in WP2, and modelling in WP3.


Ing. Lucie Pitrová Netolická has been working as a leader of the laboratory of moisture solids and metrology for two years. She is a junior research scientist with two years’ experience in moisture measurement of grain, oilseeds, wood, paper and textiles. She also has extensive knowledge of chemistry. She has been working on tasks of technology development in moisture of grain, oilseeds and wood.

Ing. Milada Racková has been head of the regional branch of the Czech metrology institute in Pardubice since 2006. She worked as a leader of the laboratory of moisture solids and metrology for 14 years. She has undertaken tasks of technology development in moisture of grain, oilseeds and wood, and volume weight since 1998. She has experience with moisture of grain, oilseeds, wood, paper and drugs. She has published 2 papers in the national magazine “Metrology”.

Radek Strnad, head of the Thermal Properties Department and senior research scientist, has worked in temperature and humidity measurement for 6 years and for 13 years in industrial metrology. He represents CMI on the EURAMET TC-T committee. He has published more than 10 papers on temperature measurement and more than 13 papers about flow measurement.

Key publications:

Strnad R., Šindelář M., The Laboratory Setup for Calibrating of the Surface Temperature Sensors, Proceeding of the Tempmeko 2010 Slovenia, page 251, ISBN 978-961-6664-02-8

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JRP-Participant 5 - DTI (funded JRP-Partner)

The Danish Technological Institute (DTI) is a self-owned and non-profit institution with about 1000 employees. It develops, applies and disseminates research- and technologically-based knowledge for the Danish and International business sector. As such DTI participates in development projects which are of use to society in close collaboration with leading research and educational institutions both in Denmark and abroad. DTI is approved by the Ministry of Science, Technology and Innovation and is the designated institute for water flow, contact temperature, geometry and anemometry, and further works with state-of-the-art measurement calibration in the fields of electrical quantities, time, mass, force, pressure, gas mixtures and humidity.

DTI has been working within drying processes, moisture measurement and testing for over 6 years. DTI has been a consultant and R&D partner for several national stakeholders in industry; for SMEs as well as major international players. These industrial stakeholders for moisture measurement have mainly been end-users, primarily with respect to drying processes and equipment manufacture. DTI disseminates knowledge nationally within an existing customer network of more than 14 000 companies. DTI provides courses, workshops and conferences for more than 30 000 participants annually on, amongst other topics, drying and moisture measurement. DTI has participated actively in EURAMET Project 1065 and hosted a “Workshop on the measurement of moisture” as a part of this work. DTI has presented its work within the fields of drying and moisture measurement at national conferences, e.g. as conference host or as part of innovation network meetings, as well as at international conferences like the Nordic Drying Conference.

In WP1, DTI will develop metrologically sound techniques for the establishment of representative primary traceability for moisture measurement equipment directly or by comparison via material samples. The work will result in a number of new services being made available for industry. More accurate and detailed measurements would further lead to better diffusion simulation models among others needed in industry for optimising drying processes.


Jan Nielsen has 20 years experience in metrology with special expertise in humidity and temperature measurement. He has a background as physicist and leads a team of 13 metrologists, engineers and physicists.

Ebbe Nørgaard has been the pioneer of DTI’s drying activities for the last 6 years and leads a team of 11 engineers, physicists and chemists. He is the project manager for several drying projects and consultancy activities.

Claus Melvad works with consultancy and R&D initiatives in moisture measurements and has disseminated knowledge within this field at national conferences and workshops.

Key publications:

J. Nielsen, C. Barendregt, “The use of thermistors for establishing the temperature conditions in a climatic chamber” (proceedings on TEMPMEKO 2004)

J. Nielsen, M. J. de Groot, “Revision and Uncertainty Evaluation of a Primary Dewpoint Generator”, Metrologia, volume 41, issue 3, pp. 167 – 172 (2004)

J. Nielsen, M. J. de Groot, “A New Set-Up for the Generation of Humidity in the ppb Range”, Proceedings on TEMPMEKO (2001)

JRP-Participant 6 - INRIM (funded JRP-Partner)

The Istituto Nazionale di Ricerca Metrologica (INRIM) is the Italian national public body tasked with carrying out and promoting scientific research in metrology. Its research activities in measurement science, materials science and innovative technologies are recognised at a worldwide level. INRIM undertakes studies and research on the realisation of primary standards for the basic and derived units of the International System of units (SI), assures the maintenance of such standards and their international comparison, and in general provides measurement traceability to the SI. In addition to physical and engineering metrology, its main R&D areas are in fundamental physical constants, materials, metrology for chemistry, nanotechnology, innovation, and quantum information.

The Thermodynamics Division of INRIM reproduces, maintains and disseminates the SI units of temperature and acoustics. It has long established experience in humidity standards and primary thermometry and, more broadly, in gas metrology. The established know-how and competences to be shared in this JRP include the development of humidity generators and measurement techniques for humidity sensing, the development of

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acoustic/microwave methods for the determination of thermodynamic temperature and for the determination of the Boltzmann constant from speed of sound measurements in helium, the development of surface temperature and air temperature standards, and the development of dielectric thermometry based on microwave whispering-gallery resonators.

INRIM’s role in the JRP will be to develop and improve present moisture meter transfer standards – suitable to insure on site traceability and to carry out laboratory intercomparisons – and to develop mathematical models relevant to moisture metrology and uncertainty analyses to underpin moisture traceability. INRIM will lead WP3.


Prof. Vito Fernicola is the Head of the Thermodynamics Division at INRIM and professor in ‘Thermal measurements and controls’ at the Politecnico di Torino. His main interests lie in measurement standards and instrumentation. He has worked on temperature standards, optical fibre and fluorescence thermometry, and industrial applications of contact thermometry. He is currently working on humidity standards and sensors. He is chair of the Italian mirror IEC SC65/B WG 5 on industrial thermal sensors. He is the Italian delegate to CIPM/CCT and member of CCT/WG6 and the EURAMET TC-T contact person.

Dr Roberto Gavioso is a research scientist acting as the Group Leader of the Physical Acoustics Program of INRIM. He leads research activities in the application of acoustic and microwave techniques to the development of novel temperature and humidity standards. His previous achievements in the field include the determination of the Boltzmann constant by two different methods.

Key publications:

Fernicola V., Banfo M., Rosso L. Smorgon D., “Investigations on Capacitive-based Relative Humidity Sensors and Their Stability at High Temperature”, Int. J. Thermophysics, Vol. 29, pp. 1668-1677 (2008)

Fernicola V., Rosso L., Giovannini M., “Investigation of the Ice-Water Vapour Equilibrium along the Sublimation Line”, Int. J. Thermophysics. DOI: 10.1007/s10765-011-1128-2 (2011)

Gavioso, R. M., Benedetto, G., Giuliano Albo, P. A., Madonna Ripa, D., Merlone, A., Guianvarc’h, C., Moro, F., Cuccaro, R., “A determination of the Boltzmann constant from speed of sound measurements in helium at a single thermodynamic state” Metrologia, 48, 387-409 (2010)

Rosso L., Koneva N., Fernicola V., “Development of a Heat Pipe-based Hot Plate for Surface-Temperature Measurements, Int. J. Thermophysics, Vol. 30, pp. 257-264 (2009)

JRP-Participant 7 - NPL (funded JRP-Partner)

The National Physical Laboratory (NPL) is the UK’s national measurement institute and is a world-leading centre of excellence in developing and applying the most accurate measurement standards, science and technology available.

Building upon comprehensive humidity capabilities established since the early 1980s, NPL has developed facilities for moisture measurement over the past 5 years, addressing moisture content in a variety of materials and sample types. Services offered include measurements, research studies, training, consultancies and instrument assessments. NPL expertise includes validation and uncertainty analysis of primary standards, and the moisture specialists have access to a large team of materials scientists within NPL. Moisture capabilities include: LoD measurements (using either the classic approach or variants of this) water-specific evolved-vapour analysis, microwave resonance analysis for rapid non-destructive measurement of bulk free water content, and extensive supporting capabilities and techniques for humidity control and measurement, for conditioning and studying water content. NPL has extensive contact with users and suppliers of moisture instruments, established through past studies of user needs.

NPL will lead WP4 (Creating Impact), and deliver tasks in WP1 on primary methods, and in WP2 on CRMs.


Dr Stephanie Bell is a Principal Research Scientist at NPL, with more than 25 years in humidity research, and 15 years involvement in moisture in materials. She chairs CIPM CCT WG6 Humidity measurements, and national standardisation committee BSI CPI 29 Humidity and temperature conditioning requirements. She leads NPL’s work on humidity and moisture, and has published more than 50 papers and reports. She is an ISO 17025 assessor for humidity laboratory accreditation, leads NPL’s humidity training course, and is a Fellow of the UK Society of Environmental Engineers.

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Paul Carroll is a Higher Research Scientist with 10 years’ experience in humidity and vacuum metrology at NPL, and 5 years specialising in moisture measurement. He has carried out measurements and research studies of moisture in a variety of materials in bulk and particulate form, using microwave, evolved vapour analysis, and LoD techniques, for biomaterials, polymers, metals, foodstuffs, and others.

Key publications

The NPL Primary Gravimetric Hygrometer, Stephanie Bell, in Papers and Abstracts from the Third International Symposium on Humidity and Moisture, 1998, Volume 1, pp. 20-27. ISBN 0 946 754 24 1

Non-destructive moisture content measurement of bioabsorbable polymers used in medical implants P.A. Carroll, S.A. Bell, A.S. Maxwell, P.E. Tomlins, International Journal of Thermophysics DOI: 10.1007/s10765-011-0981-3, Published online 1 May 2011

G. Hinds, M. Stevens, J. Wilkinson, M. de Podesta, S. Bell, Novel in situ measurements of relative humidity in a polymer electrolyte membrane fuel cell, Journal of Power Sources, 186 (2009) 52-57

Outgassing of water vapour, and its significance in experiments to determine the Boltzmann constant Michael de Podesta, Gavin Sutton, Robin Underwood, Stephanie Bell, Mark Stevens, Thomas Byrne and Patrick Josephs–Franks. Metrologia 48 L1 (2011) doi: 10.1088/0026-1394/48/1/L01

JRP-Participant 8 - TUBITAK (funded JRP-Partner)

As the National Metrology Institute of Turkey, TUBITAK UME, officially established in 1992 as a separate institute, operates with the mission to establish national measurement standards for providing traceability to the secondary level laboratories. The institute carries out research, especially focusing on measurement device producer companies, raw materials producers, industrial automation, military and advanced energy technologies.

The TUBITAK UME Humidity Laboratory is a primary level humidity laboratory that has been functioning for 13 years. Calibration of moisture meters, psychrometers and humidity chambers are performed amongst other calibration tasks of the laboratory. TUBITAK has participated in major EURAMET and CCT-key comparisons and intends to establish primary standards for moisture. The TUBITAK UME Humidity Laboratory has a climatic chamber, a two-pressure humidity generator, and equipment for the LoD technique. TUBITAK UME also has the ability to measure moisture in solid materials with Karl Fischer and TGA-MS devices. Dielectric and microwave techniques to make measurements of moisture in materials are the other abilities of TUBITAK UME.

TUBITAK will be involved in WP1, with the studies on realisation methods for moisture in plastic and paper materials in sheet form. In WP2, TUBITAK will contribute to the research on handling and transportation of samples, transfer standards, and calibration methods for surface moisture meters. In the modelling development work of WP3, TUBITAK’s focus is on moisture diffusion in paper sheets.


Seda Oğuz Aytekin has been working in the temperature laboratory since 1995 and was involved in the foundation of the humidity laboratory in 1999. She is the main responsible person in humidity calibrations and intercomparisons. She is a member of CCT WG6 and the contact person of TUBITAK UME for the humidity subcommittee of EURAMET TC-T.

Ali Uytun has been working in the temperature laboratory for 14 years. He has been dealing with humidity measurements for more than 10 years. He is also involved in research on the triple point of water. He recently got his Master of Science degree by preparing his thesis on soil moisture measurement. He has published several papers in this field in Turkey.

Key publications

Uytun A., Kartal Dogan A., “Islaklık Ölçümleri (Moisture Measurements) ”, VII. Ulusal Ölçüm Bilim Kongresi – VII. National Metrology Conference, 2008, İzmir

Ali UYTUN, Beyhan PEKEY, Emrah UYSAL, Oktay CANKUR, Aliye KARTAL DOĞAN, " Kocaeli Kentinde Seçilen Kırsal Bölgelerde Toprak Kirliliğinin Araştırılması (Investigation of Impurities in Soil in Kocaeli District", 9. Ulusal Çevre Mühendisliği Kongresi – 9

th National Environmental Engineering Conference, 05-08

October 2011, Samsun

Ali Uytun, "Kocaeli Kentinde Seçilen Kırsal Bölgelerde Toprak Nemi ve Toprak Kirliliğinin Belirlenmesi - Investigation of Impurities in Soil and Soil Moisture in Kocaeli District ", Master of Science, Kocaeli University, 2012, Kocaeli

http://www.springerlink.com/content/0195-928x/

http://dx.doi.org/10.1088/0026-1394/48/1/L01

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JRP-Participant 9 - UL (funded JRP-Partner)

The Laboratory of Metrology and Quality (LMK) at the Faculty of Electrical Engineering (FE), University of Ljubljana (UL, Slovenian: Univerza v Ljubljani – legal entity) is a Designated Institute under the National Metrology Institute of the Republic of Slovenia (MIRS). The laboratory (MIRS/UL-FE/LMK – classification according to EURAMET as associate member and DI of the Metrology Institute of the Republic of Slovenia, MIRS) is a holder of a national standard of thermodynamic temperature and humidity. There are 13 members of the LMK. The laboratory’s calibration measurement capabilities (CMC) in the field of thermometry and hygrometry are comparable with the best similar capabilities of European countries and other countries, and currently it contains 45 CMC BIPM database entries. The laboratory’s main research activities are oriented to the new fields of fundamental metrology, especially to contact and non-contact thermometry and hygrometry. In the field of hygrometry the MIRS/UL-FE/LMK has developed a primary humidity generator with performance in the top level of the European standards and carried out research on dew/frost formation in dew-point sensors and psychrometers. MIRS/UL-FE/LMK assures traceability for temperature and humidity measurements to a range of demanding industrial partners, which has resulted in several research joint and traceability projects.

In the field of moisture transport LMK has conducted a study of water vapour permeation through materials. The laboratory also manages and hosts a website in the scope of EU FP5 project Incolab, EU FP6 project Minet, in the scope of joint international symposium Tempmeko & ISHM in 2010 and JRP ENV07 MeteoMet. Within MeteoMet LMK also leads tasks on protocols for quality assessment of ground-based measurement and software validation of in situ weather stations.

UL will develop a novel calibration system for surface moisture meters in WP2 and contribute to the experimental validation of moisture models in WP3.


Prof. Janko Drnovšek is head of the LMK. He has been involved in thermal metrology for more than 30 years as researcher. He is an author and co-author of more than 40 published research SCI papers.

Dr. Domen Hudoklin has 15 years of research experience in hygrometry. He is in charge of humidity measurements in the LMK and is responsible for maintaining a humidity primary standard. He is an author and co-author of 10 research SCI papers.

Dr. Gaber Beges has 15 years of research experience in testing. He is in charge of safety testing of electrical appliances and his research work is mainly devoted to the development and evaluation of test methods and interlaboratory comparisons. He is an author and co-author of 11 research SCI papers.

Key publications

Hudoklin D., Bojkovski J., Nielsen J., Drnovšek J., “Design and validation of a new primary standard for calibration of the top-end humidity sensors”, Measurement [Print ed.], vol. 41, no. 9, pp. 950-959 (2008)

Hudoklin D., Barukčić E., Drnovšek J., “Engaging frost formation in a chilled-mirror hygrometer”, Int. J. Thermophys., vol. 29, no. 5, pp. 1598-1605 (2008)

Kentved A. B., Heinonen M., Hudoklin D., “Practical Study of Psychrometer Calibrations”, Int. J. Thermophys., accepted for publication (2012), DOI: 10.1007/s10765-012-1212-2

Hudoklin D., Setina J., Drnovsek J., “Uncertainty Evaluation of the New Setup for Measurement of Water-Vapor Permeation Rate by a Dew-Point Sensor”, Int. J. Thermophys., accepted for publication (2012), DOI: 10.1007/s10765-012-1213-1

JRP-Participant 10 - UT (funded JRP-Partner)

UT, University of Tartu, is the largest university in Estonia. Metrology in chemistry is a core research and education direction at UT. This is witnessed by a number of scientific publications, DI status of UT in Estonia (metrology in chemistry, air humidity, air flow), participation in iMERA Plus and EMRP projects (T2J10 Tracebioactivity, ENG09 Metrology of Biofuels and ENV05 Oceans), running an international Master's programme "Applied Measurement Science" (http://www.ut.ee/ams/), and initiating a pan-European metrology-in-chemistry consortium "Measurement Science in Chemistry" (http://www.msc-euromaster.eu/) UT has a metrology-oriented unit - Testing centre - accredited according to the ISO 17025.

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In connection with its DI status UT carries out research in moisture metrology in the gas, liquid and solid phases. Coulometric KF titration is the main technique that UT uses in liquids and solids and this technique is one of the two primary techniques that will be elaborated in this project.

UT will carry out research into cKF as a realisation method for moisture in WP1 and will contribute to the development of CRMs and model uncertainty analysis in WP2 and WP3, respectively.


Prof. Ivo leito has metrology in chemistry among his core research areas. He has published close to 100 papers indexed by the Thomson-Reuters Web of Science. About half of them are related to different chemical measurements and their metrological aspects. He is also a Europe-wide active educator in Metrology in Chemistry.

Dr Lauri Jalukse works in metrology of chemistry as one of his core research areas. In 2007 he defended his PhD thesis, which was fully dedicated to metrological investigation of another titration technique – the Winkler titration.

Key publications

I. Helm, L. Jalukse, I. Leito: A highly accurate method for determination of dissolved oxygen: Gravimetric Winkler method. Anal. Chim. Acta 741 (2012) 21-31, http://dx.doi.org/10.1016/j.aca.2012.06.049

K. Kaupmees, I. Kaljurand, I. Leito: Influence of Water Content on the Acidities in Acetonitrile. Quantifying Charge Delocalisation in Anions J. Phys. Chem. A 114 (2010) 11788-11793

I. Helm, L. Jalukse, I. Leito: Measurement Uncertainty Estimation in Amperometric Sensors: A Tutorial Review, SENSORS 10 (2010) 4430-4455

L. Jalukse, I. Helm, O. Saks, I. Leito: On the accuracy of micro Winkler titration procedures: a case study Accreditation and Quality Assurance 13 (2008) 575-579

JRP-Participant 11 – UNICLAM (REG)

The REG is funded and contracted directly by EURAMET, however the REG-Researcher will report to the JRP-Consortium in terms of tasking and progress.

UNCLAM is involved in several research topics such as energetic, thermo-fluid-dynamic, heat transfer, thermal comfort, metrological, and environmental measurement issues. In particular, the researchers apply both experimental and Computational Fluid Dynamics (CFD) approaches to study complex case-studies like velocity field measurement in local ventilation systems, mass and energy transfer in porous media (design of geothermal heat exchanger, modelling of reactant gases in porous electrodes of fuel cells), thermal fluxes in the proximity of complex systems (combustion chambers, climatic chambers, fuel cells,…), and exposure to airborne particles in different microenvironments (both indoor and outdoor microenvironments). As regards the CFD approach, the Home Organisation of Cassino proposed and validated a non-commercial numerical code able to deal with laminar and turbulent incompressible flows, both stationary and non-stationary, flowing whether in free or porous media, by considering both two- and three-dimensional domains. The metrological skills of the Home Organisation include mechanical (mass, length, force) and thermo-fluid-dynamic (temperature, pressure, flow rate, thermal flux, volume, laser-based velocity measurement techniques such as PIV) measurements. The metrological activity is focused on the design of complex measurement techniques and the evaluation of their uncertainty budgets.

UNICLAM will develop numerical modelling and contribute to the validation of the models in WP2.


Gino Cortellessa (named researcher) gained his masters degree in Mechanical Engineering at the University of Cassino in 2009. In 2009 he was awarded a contract for the identification of an innovative methodology for analysing energy system planning, research carried out under agreement with the province of Frosinone. Winner of the competition for admission to a PhD school in mechanical engineering at the University of Cassino in the academic year 2009/2010, he is mainly interested in issues related to numerical models of porous media in transient regime and multiscale modelling of heat conduction.

Marco Dell'Isola is Full Professor at the University of Cassino and Lazio Meridionale (UNICLAM). From 2004 to 2011 he was Deputy Dean of the Faculty of Engineering of Cassino and Chairman of the Doctoral Program in Mechanical Engineering; he was the delegate of the Rector of the University for energy issues; responsible for the university accredited centre and for the Laboratory of Industrial Measurements (LAMI). He was Deputy Director of the DIMSAT (Department of Mechanics, Structures, Environment and Territory).

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Since 2012 he has been Director of the Department of Civil Engineering and Mechanics and a member of the Academic Senate of the University. His research activities mainly refer to the areas of energy and environmental sustainability as well as the metrology of thermofluidodynamics quantities.

Key publications

M. Dell’Isola, F. R. d’Ambrosio Alfano, G. Giovinco and E. Ianniello, Experimental Analysis of Thermal Conductivity for Building Materials Depending on Moisture Content, Int. J. Thermophys., 2012, DOI: 10.1007/s10765-012-1215-z

G. Buonanno, M. Dell’Isola, L. Stabile, A. Viola, Critical aspects of the uncertainty budget in the gravimetric PM measurements, Measurement, Vol. 44, Issue 1, January 2011, 139–147

F. Arpino, M. Dell’Isola, G. Ficco, L. Iacomini and V. Fernicola, Design of a Calibration System for Heat Flux Meters, Int. J. Thermophys., Vol. 32, Numbers 11-12 (2011), 2727-2734

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Section G: Collaborators

These collaborators do not deliver work content of the JRP, do not sign the JRP-Contract and are not bound by its terms and conditions. The relationship between each collaborator and the JRP-Consortium will be addressed through an ‘Exchange of Letters’

The organisations below have indicated their potential willingness to collaborate with the JRP in areas of mutual interest.

Short name Organisation legal full name

Country Area of collaboration

(WP number and detail)

Raute Raute Oyj Mecano Business Unit

Finland WP2: Provide plywood samples and perform measurements with industrial equipment

WP4: Provide information on the industrial needs related to reference measurements in plywood production

Metrohm Metrohm Nordic Oy

Finland Instrument manufacturer – electrochemical analytical instruments incl. cKF

WP1, WP4: advice

Metso Metso Automation Inc.

Finland WP1 & WP2: Loan an NMR moisture analyser for studying samples

WP4: Provide information on the needs of process instrument manufacturer for calibrations and contribute to the workshops

Mettler-Toledo

Mettler-Toledo AG

Switzerland Instrument manufacturer – analytical instruments

WP1, WP4: advice

RCL Rubislaw Consulting Ltd

United Kingdom

Industrial consultancy – fish technology

WP1, WP4: advice

Intertek ITS Testing Services, Ltd (Intertek Pharmaceutical Services Manchester)

United Kingdom

Contract research organisation – pharmaceuticals, biopharmaceuticals, medical devices

WP1, WP2, WP4: advice

LGC LGC Limited United Kingdom

UK Designated Institute for chemical metrology, and measurement research laboratory

WP1, WP2, WP4: collaboration on CRM development

UCL University College London (School of Pharmacy)

United Kingdom

University – Pharmaceutics


Henkel Henkel Slovenija d.o.o.

Slovenia Manufacturer of adhesives

WP2, WP4: advice

Seltek Seltek Ltd Turkey Instrument supplier – tobacco, food, concrete, chemicals, brick etc.

WP2, WP4: advice

MSL The Measurement Standard Laboratory of New Zealand

New Zealand

National Metrology Institute

WP4: advice

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UNIIM The Ural Research Institute for Metrology

Russia Designated institute – moisture in food, grain, compound feed, fertilisers, pharmaceuticals, hardwood, coal, polymers, concrete


VNIIM D.I. Mendeleyev Research Institute for Metrology

Russia National metrology institute – moisture in wood, construction materials

WP2, WP4: advice

PTB Physikalisch-Technische Bundesanstalt

Germany National metrology institute – moisture in grain and oilseeds


KRISS Korea Research Institute of Standards and Science

Republic of Korea

National metrology institute – moisture in wood, paper, construction materials, soil

WP1, WP2, WP3, WP4: advice

NIST National Institute for Standards and Technology

USA National metrology institute – CRMs

WP2, WP4: advice

Section H: References

[1] S. Bell, R. Benyon, N. Böse, M. Heinonen, A roadmap for humidity and moisture measurement, Int. J. Thermophysics 29 (2008) 1537-1543

[2] V. Fernicola et al., A European roadmap for humidity and moisture, 2012, www.euramet.org

[3] P. A. Carroll, S. A. Bell, Consultation on the use of certified reference materials for the calibration of moisture measurement instrumentation NPL Report ENG 40. 2012.

[4] http://www.euramet.org/index.php?id=1755

[5] B. Joseph, T. Le Goff, Validation of the Metrohm 774 Oven Sample Processor and 831 Karl Fischer Coulometer for Moisture Determination. LGC report LGC/AT/2006/019, 2006.

[6] Certified Reference Materials 2012, EU Joint Research Centre IRMM, 2012, 78p

[7] http://www.nist.gov/srm

[8] Report of the 17th meeting Consultative Committee for Amount of Substance: metrology in chemistry (CCQM) to the International Committee for Weights and Measures, www.bipm.org/utils/common/pdf/CCQM17.pdf

[9] Report A917-30, World Physical Properties Instrumentation Markets, Frost and Sullivan, 2006

http://www.nist.gov/srm

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