metefnet m24 presentation v2 mh150515...

Metrology for Moisture in Materials

SIB64 METefnet2nd General Project Meeting

Martti Heinonen, Maija Ojanen-Saloranta, Stephanie Bell, Vito Fernicola, Eric Georgin, Gino Cortellessa

CETIAT, Lyon, France16 June 2015

Version 2.0

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Agenda09:00 – 09:15 Opening09:15 – 09:30 Participants, meeting aims and objectives09:30 – 09:50 WP5: Management and Coordination09:50 – 10:05 REG210:05 – 11:00 Progress in WP411:00 – 11:15 Coffee break11:15 – 12:45 Progress in WP112:45 – 13:45 Lunch13:45 – 15:15 Progress in WP2 15:15 – 15:30 Coffee break15:30 – 16:45 Progress in WP3 + REG116:45 – 17:00 Close of meeting17:00 – 19:00 Visit to laboratories at CETIAT

Participants, meeting aims and objectives• Participants:

• List

• Introduction of collaborator representatives

• Aims and objectives:• Briefly review the progress within the first 12 months

• Highlights and potential problems

• Plan the work in the next 12 months (until the end of project)

• Collaboration: in protocol and new ideas

• Work with collaborators

• Enhancing the impact

• Deepen the coordination and identity of the European moisture metrology3

WP5: Management and Coordination• Reporting:

• M18:• Comments of MSU not yet arrived

• Feedback from mid-term review

• M24:• Input to WP leaders (and MIKES) by 8 June 2015

• WP leader reports to MH (& KN) by 24 June 2015

• MH will submit the report on 29 June 2015!!

4

WP5: Management and Coordination• Meetings:

• PMB: • 1st net meeting was on 15th November 2013

• 2nd net meeting: 4th November 2014

• 3rd net meeting: November 2015

• GPM• 1st meeting at BRML on 3rd to 4th June 2014

• 2nd meeting at CETIAT on 16th 2015

• Other• Task1.1 / net meeting: 3rd September 2014

• Final meeting at DTI: May 2016

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WP5Collaborators

6

1 RauteRaute Oyj Mecano Business Unit Finland EoL OK

2 Metrohm Metrohm Nordic Oy Finland

3 UPTCUniversidad Politécnica de Cartagena Spain

EoL in process

4 Valmet Valmet Automation Inc. Finland EoL OK Note: new name of Metso

5Mettler-Toledo Mettler-Toledo AG Switzerland

6 RCL Rubislaw Consulting Ltd UK

7 Intertek

Intertek Pharmaceutical Services Manchester, ITS Testing Services, Ltd UK EoL OK

8 LGC LGC Limited UK

9 UCL UCL School of Pharmacy UK

10 Henkel Henkel Slovenija d.o.o. SloveniaEoL in process

11 Seltek Seltek Ltd Turkey EoL OK

12 MSLThe Measurement Standard Laboratory of New Zealand New Zealand

13 UNIIMThe Ural Research Institute for Metrology Russia EoL OK

14 VNIIMD.I. Mendeleyev Research Institute for Metrology Russia

15 PTBPhysikalisch-Technische Bundesanstalt Germany

16 KRISSKorea Research Institute of Standards and Science Korea

EoL in process

17 NISTNational Institute for Standards and technology USA

18 NIMT

National Institute of Metrology, Thermometry Metrology Department Thailand

EoL in process

19 Novasina Novasina AG Switzerland

20 NISNIS - National Institute for Standards Egypt EoL OK Proposal for comparison

21 Domel Domel d.o.o Slovenia EoL OK

REG2: Research in moisture measurement instruments (RIMMI)• Status & plans for M24 to M36

7

REG2: Deliverables

8

No Description Original Actual Status & NotesREG D2 Measurement set-ups

built May 14 Sept 14

REG D3 Measurement results of repeatability and reproducibility obtained

Sep 14 Jan 15

REG D4 Comparison with results from oven drying method carried out

Sep 14 Jan 15

REG D5 Initial measurements May 15 Oct 14

REG D6 Measurement results for at least five different materials

Jul 15 Jul 15

REG D7 Measurement results on the effect of material properties

Nov 15

REG D8 Comparison with reference measurements

Dec 15

REG D9 Measurement results on the effect of ambient conditions

Feb 16

Progress in WP4• Status & plans for M24 to M36

• Collaboration with collaborators

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WP4: Creating impactOverview at M24:

No. Report no. of items reported (auto filled)

1 STANDARDS & REGULATORY ACTIVITIES (STAN) 122 PUBLICATIONS (PUB) 73 CONFERENCE PRESENTATIONS & POSTERS (CONF) 134 TRAINING (TR) 115 OTHER DISSEMINATION (OTH) 276 FOLLOW‐ON COLLABORATIONS (FOLL) 07 END USER UPTAKE & EXPLOITATION (UP) 08 COLLABORATORS & STAKEHOLDERS (COLL) 349 APPLICATIONS FOR PATENTS, TRADEMARKS, REGISTERED DESIGNS (IP) 010 EXPLOITABLE FOREGROUND, ETC (FG) 011 FUTURE EVENTS (FUT) 4

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WP4: Creating impact• Main steps in the next 12 months (to end of project):

• Continue with deliverables already running

• D4.2.1 Training course (some progress – and report –scheduled for Nov 2014) CETIAT, UT, DTI

• D4.2.2 We said workshops would be delivered Nov 14 and May 15 (and others later) CETIAT, INRIM, MIKES,TUBITAK,REG (UNICLAM)

− Will they be?

• Issues in collaboration with partners and collaborators:• Not all collaborators have signed a letter agreement. If they

don’t we can’t count them in the numbers for the project

12

D4.1.1 Liaison with stakeholders though two-way sharing of information, by correspondence, meetings and visits (All)• Such as:Visit to the paper mill "Cartiere di Guarcino SpA.", May

2015 UNICLAM

• Probably others … are they in the Impact spreadsheet?

WP4: Creating impact – active work

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D4.1.2 Website UL (and all)• Web site fully functional and updated. Online calendar of

events.• Also – announcements on other web pages (Announcing

METefnet workshop on CETIAT and Metrologie Françaiseweb page … (others?)


14

D4.1.3 Active input and dissemination though sector technical and standards committees NPL, INRiM, DTI

In the last six months:

• BIPM CCQM IAWG• EURAMET TC-T Humidity • Engagement (NPL) with BSI committees

• AW/4 Cereals and pulses• CII/37 Fertilisers and related chemicals• AW/8 Tea• PRI/82 Thermoplastic materials• NFE/36 Copper lead and zinc ores and concentrates• PTI/16 Solid mineral fuels

• Others?


15 Are we still targeting these ones?

16

D4.1.4 At least 5 presentations at conferences, presenting overview or individual outputs of the project MIKES, BRML, CETIAT, DTI, NPL, REG (UNICLAM) • Target already achieved at TEMPMEKO 2013 ☺• REG(UNICLAM)

• Transient incompressible flow in a partially porous buoyancy driven tall cavity ASME-ATI-UIT 2015, May 2015, Italy

• UL• Development of a sensor for measuring surface moisture,

Seminar on optic communications, February 2015, Slovenia

D4.1.5 At least 5 paper or electronic publications spanning trade magazines, sector-specific and measurement journals DTI, BRML, CETIAT (and others?)• None this six-month period? • But target of 5 already exceeded ☺


17

WP4: Creating impact

Submission deadline 3 July!

Draft some time before that (so make sure M24 details are ready before then).

18

The following are, or should be, “in progress”

D4.1.6 Guide on Karl Fischer Titration usage and uncertainty evaluation UT, due Sep 2015

D4.2.1 Develop new training course material and case studies CETIAT DTI, UT – due Apr 2016

D4.2.2 Workshops (scientific and/or training) CETIAT, INRIM, MIKES,TUBITAK, REG (UNICLAM) – due by May 2016

• Tomorrow is one of them

• 3D printer Training, April 2015, Italy, REG(UNICLAM)

• Plus 10 other training events so far - UNICLAM, INRIM, NPL, UT, CETIAT

WP4: Creating impact – work started

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D4.2.3 Two-way training during guestworking REG(UNICLAM),DTI

- Due by April 2015

D4.3.1Two-way liaison with relevant groups in IMEKO, EURAMET and other RMOs, and relevant CIPM CCs NPL, All• Several throughout the JRP• This period:

• EURAMET- TCT Feb 2015• CCQM IAWG Apr 2015

• Discussion document submitted to meeting of IAWG• There is more to do - we can prepare other actions ….

WP4: Creating impact – work started

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Others – are these started?

D4.3.2 Report proposing future actions on international metrological infrastructure for moisture metrology NPL, All, by Mar 2016

• not started

D4.4.1 New/improved calibration, sampling and measurement services BRML, DTI, MIKES, NPL, TUBITAK

• ?

D4.4.2 Extend upon existing consulting services INRIM, DTI, MIKES• By May 2015?

D4.4.3 Report on the exploitation route for new CRM(s) developed during the project NPL, BRML, UT

• not started

WP4: Creating impact (action soon)

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Remember: only publications carrying the following acknowledgment can be counted as EMRP project delivery:

The EMRP is jointly funded by the EMRP participating countries within EURAMET and the European Union.

WP4: Creating impact (future)

WP4: Deliverables in Task 4.1

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No Description Original Actual Status & Notes4.1.1 Liaison with stakeholders May 14

May 15May 16

May 14 In progress

4.1.2 Website Every 6 months

Every 6 months

In progress

4.1.3 Active input and dissemination though sector technical and standards committees

May 14May 15May 16

May 14 In progress

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

May 14Nov 14Sep 15Nov 15

May 14Nov 14

Target achieved. More in progress/planned.

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

May 14May 15Apr 16

May 14 Target achieved. More in progress/planned.

4.1.6 Guide on Karl-Fischer titration usage and uncertainty evaluation

Sep 15 ?

WP4: Deliverables in Tasks 4.2 to 4.4

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No Description Original Actual Status & Notes4.2.1 Develop new training course

material and case studies Nov 14Apr 16

Nov 14 ?

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

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

Nov 14 In progress?

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

May 14May 15May 16

May 14 In progress. Further work planned.

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

Mar 16 Not started

4.4.1 New/improved calibration, sampling and measurement services

Nov 14Mar 16

Nov 14 In progress?

4.4.2 Extend upon existing consulting services

May 15 In progress?

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

Apr 16 Not started


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Progress in WP1• Task 1.1

• D1.1.7 ongoing: Measurements made/ongoing with pellets (DTI, NPL, MIKES, UT, INRIM), forest based biomass (MIKES), paper(BRML, TUBITAK?), polymer sheet, milk powder, fructose, tealeaves (INRIM), wood (CMI), foodstuff, pharmaceuticals (NPL)…

• Methods (compared with LoD): Evolved vapour technique(NPL), cold trap (MIKES), cKF (UT, INRIM), chilled mirror (DTI), TGA (TUBITAK)

• Dataset to be collected by September 2015. Please send yourresults to Martti!

• Delays in publications (D1.1.5, D1.1.6), but they will be submittedsoon, and do not cause delays on other deliverables

• TUBITAK & others: Plan for D1.1.8 (Peer-reviewed journal or conference paper on uncertainty estimation tools for gravimetric SI moisture unit realisation submitted) ?

26

Progress in WP1• Task 1.2

• D1.2.3 and D1.2.4 are delayed, as work at BRML was delayed for 6 months. In D1.2.4, The cKF method has been developed. Compiling the method description is in progress and will be delivered shortly.

• Plan to finalize the deliverables?

• D1.2.5 Validation report and uncertainty budget available for the cKF method, due July 2015. Will this be delayed too?

27

Progress in WP1• Task 1.3.

• D1.3.1. Report on the review of terms and definitions in moisture measurements by NPL, due May 2015. What is the status?

• Preparation for comparisons?

• D1.3.2 (cKF/LoD, polymeres, UT, BRML, TUBITAK)

• D1.3.3 (Foodstuff and biomass, MIKES, BRML, CETIAT, DTI, NPL, TUBITAK)

• D1.3.4 (CRMs developed in WP2, NPL, DTI, TUBITAK, BRML)

• Collaboration with collaborators

• MIKES received plywood samples from Raute. These samples are used to study dry materials and effects of crushing. Meeting with Finnishstakeholders in September 2015.

• TBD Biodiscovery has supplied a chemical (its identity cannot be disclosed) of interest to UT and as a result there is now a reliable moisture determination procedure available.

• MIKES received a calibration inquiry for IR dryer moisture meter

• Training and workshops: INRIM, DTI28

WP1: Preliminary intercomparison with pellets (JN)

• Objective: • A preliminary validation of the developed standards (target uncertainty:

0.5 % to 4 % depending on method)

• Method• Commercial wood pellets sampled, packed and distributed by DTI

• Main troublemakers at 105 °C measured with gas-chromatograpy to be: Acetone, Acetic Acid and Pentanal

• Total VOC’s measured using Photo-Ionization-Detection to approx 200 ppm

• At higher temperatures (<200 °C): Hexanal (bp 130 °C) and Terpenes (bp155 °C – 176 °C) could cause trouble.

• Data from participants• Different methods: LoD, cKF, Vapor detection, water trap, thermal

gravimetric analysis, NIR

• Samples 1 mg – 240000 mg

• Both grinded/bulk material measured

• Analysis method used: robust according to ISO 13528:2005 … and Cox (Metrologia 2001, 39, 589-595) – but results are NOT normal distributed

• OK agreement with traditional LoD

• Water-detection method produces significantly higher values than cKF, maybe due to the handling of the samples (grinding) in cKF.

• In general quite good agreement between labs using cKF and between labs using water detection techniques

±1 % k=2

Input to the real intercomparisons to come• Consider reporting format

• An uncertainty table would be helpful

• Consider the method for calculating a reference value on beforehand

• Homogenity/stability tests of material to be tested must beperformed on beforehand

• Analysis of VOC emmisions to be done at beforehand

• Packaging material (permeability to water) is important

• Sampling and sample handling is a very important issue

Monitoring of:Efficiency of the desiccant systemStability of the background

Drift and background current

Evolved Water Vapour (EWV) Preliminary Analyses

Desiccant system working properly Desiccant system exhausted

Analysis of wood pellet

MEASUREMENT PROCEDURE:• Small amounts of sample (around

5 mg) requiredmechanical grinding of wood pellet

• Blank analysis• Calibration of the analyser by

means of the reference material: Hydranal Water Standard KF‐Oven at different water content levels (3‐point calibration curve by Weighted Least Squares)

Analysis of wood pellet at increasing temperature (at 110 °C, 150 °C and

220 °C)

LoD Temp.

Optimal Temp.

for wood samples

Cellulose degradation

High measurement repeatability due to the homogeneity of the samples- WDS: fragmented sample (smaller sheets) causes more dispersion- cKF: the sample is a unique sheet of around 10-15 cm2 having a

mass of 80 mg

Sample homogeneity

Analysis of bio‐plastics

Coulometric Karl Fischer (cKF) titration

• Chemical direct method• Chemical reaction selective for water

• Overall reaction:3Z+ROH+SO2+I2+H2O 3ZH++ROSO3

‐+2I‐

where Z is a base and ROH is an alcohol (usually methanol)

• The consumption of iodine, which is stoichiometrically equivalent to the water present in the sample, is measured

• In the cKF, iodine (I2) is formed from iodide (I‐) in the titration cell by anodic oxidation.

cKF apparatus at INRIM

Moisture measurement range: 2 ppm – 5 %

Titration cell equipped with diaphragm electrode Autosampler

Oven

Solid samples are heated in an oven and the volatile compounds are

carried into the KF titration cell for selective water determination

Development of metrologically traceable procedures

• Preliminary analyses and monitoring of the instrumental parameters

• Operational temperatures: 110 °C (pellet, bioplastic), 220 °C (reference material)• Determination of the end point of the reaction• Drift value (flux of water coming from the ambient air) and background current• Choice of the pre‐treatments of the samples

• Metrological traceability

• Use of certified mass standards for the determination of the sample masses• Calibration by means of a suitable reference material• Evaluation of measurement uncertainty

Preliminary analyses and sample preparation

• End point determination

• Fixed time: typically suggested in literature for solid samples drawback: it requires long times of analysis

• Relative drift: typically suggested in literature for liquid injectable samples advantage: it requires lower measuring times (it is useful for calibration and samples analysis)

• Problems• Sample homogeneity• Risk of contamination• Pellet pre‐treatment:

manual crushing or mechanical grinding

• Bioplastic is more homogeneous andit requires less manipulation with respect to wood pellet

Figure: crashed (left) and grinded (right) pellet samples

Figure: pellet measurements with cKF (T = 220°C)

REGRESSION ALGORITHM• Weighted Total Least Squares

(WTLS)• Uncertainty evaluation both for x

and y• Covariances• The regression was carried out by

means of CCC software developed at INRiM (MATLAB)

CALIBRATION PROCEDURE• 9 measurements with 3 different

masses of reference material at 220 °C for 15 minutes

• 3 different amounts of water measured by the instrument

Calibration of cKF

X: Crushed

●: Grinded

Loss‐on‐Drying

MEASUREMENT PROCEDURE• Use of a Termobalance Sartorius

MA150 for termogravimetric analysis• Check of the balance performances (at

ambient temperature) before each analysis by weighing calibrated mass standard mass value of 1 g and 0.9 g

• Analysis of sample aliquots around 1 g (previously weighed on an analytical balance by comparing the samples with calibrated mass standards (double substitution scheme)

• Check of the termobalance performance at the end of each analysis (at ambient temperature)

6,60%

6,80%

7,00%

7,20%

7,40%

7,60%

7,80%

Wat

er c

onte

nt (%

)

MA150cKF c30WDS 400

LoD

cKFWDS

Comparison between LoD, cKF and WDS results for wood pellet at 110 °C (bag 1). The expanded uncertainties are the standard deviations of repeated measurements multiplied by k=2

WP1: Deliverable in Task 1.1

41

No Description Original Actual Status & Notes1.1.1 Summary report on key findings of

literature reviewNov 13 Feb 14 Completed

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

May 14 July 14 Completed

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

Nov 14 A first draft of the peer-reviewed journal paper has been written and it is currently being refined. Completion is planned by end of December 2014. It is proposed to submit the paper to Metrologia.

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

May 14 May 14 Completed

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

Nov 14 Delayed to July 2015

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

Nov 14 Delayed to June 2015, due to minor problems in the measurement system and lack of personnel resources

1.1.7 Comparison data between the SI traceable moisture realisations and relevant standardised moisture determinations

May 15 Delayed to September 2015. Measurements are being performed. Collection of the dataset to be done.

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

Mar 16


42

No Description Original Actual Status & Notes1.2.1 Literature survey of the factors

determining the uncertainty of cKF method and their contributions

Sep 13 Sep 13 This deliverable is completed.

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

Mar 14 May 14 This deliverable is completed.

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

Sep 14 This deliverable is delayed to March 2015

Work at BRML is delayed for 6 months as for the measurements of powder samples will be used a titrator with oven from a collaborator of the project.

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

Jan 15 Due to the delay in D1.2.3, this deliverable is expected to be delayed to May 2015.@The OcKF method has been developed. Compiling the method description is in progress and will be delivered shortly.

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

Jul 15


43

No Description Original Actual Status & Notes1.3.1 Report on the review of terms and

definitions in moisture measurements

May 15 ?

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

Nov 15 This deliverable is on target. The polymers are available and we hope to send them in Aug 2015 to the partners.

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

Jan 16

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

Feb 16 This deliverable has not yet started.

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

Jan 14 Jan 14 This deliverable is completed.

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

Mar 16 This deliverable has not yet started.

Progress in WP2• CETIAT

• Deliverables:• Design of resonant or non resonant coaxial cells for RF/MW

transfer standard instrument (D2.3.1)

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

• Complete RF/MW transfer system with initial tests (D2.3.3)

• Experimental cell designed and machined• Capacitive cell: 1 structure 1 sample holder for solid + 1 sample

holder for liquid

• Coaxial cell: 4 structures + 1 sample holder for solid + 1 sample holder for liquid

• New people• Sébastien HUBERT (permanent position)

• Mohamed Wajdi BEN AYOUB (PhD student)44


• Capacitive cell / for solids and for liquids

45mica/silicone

RF electrode

quartz cell

LiquidGround electrode

RF electrode

N connectorTeflon

mica/silicone

Solid samples cell


• Capacitive cell / liquid cell results / electrical description

46


• Capacitive cell / resonant structure

47


• Coaxial cell

48

Samples

Samples

1"5/8coaxial lineSliding short circuit


• Thermo-coulometric water content measurement• easyH2O BERGHOF

• Drying oven method + P2O5-sensor => coulometric titration

• Temperature range: ambiant up to 400°C

• Moisture range: from 0,01% up to 15%

• Sample weigh: from 2 mg up to 2000 mg

• easyH2O can analyze different bonding form: chemically bonded water, physically bonded water and free liquid water

49

Progress in WP2• CMI

50

Progress in WP2• INRIM

• Portable humidity generator upgrade (D2.3.6)shell-and-tube h/e saturator

51

Portable temperature block calibrator

Heated hose

To Process

Ref PRT

Saturator

Pre-dryer

Am

bien

t A

ir

Diaphragm Pump

Pre-saturator


• Portable humidity generator upgradeSystem performance

52

Comparison vs a calibrated CMH: -15 ° to 50 °C dp- Temperature gradient: < 0.2 °C max- Short immersion depth: 140 mm- Flow rate: < 2 L/min


• Microwave moisture meter (D2.3.5)

53

a VNA analyzer was used to record microwave data

Tests with cylindrical microwave resonators with different aspect ratios

cavity resonances span the frequency range (2.8 GHz to 11 GHz)

40.4 mm

12.6 mmPolystyrene sample holder

• to contain moist samples under test,simple polystirene cylindricalholders were used

• teflon holders are currently beingdesigned to be gas-tight fortransportation of samples to andfrom the laboratory to test sitespreserving their original moisturecontent

moist tobacco flakes

Microwave spectrumTE modes – empty cavity

42 mm

60 mm

sample under test

antennas

TE 111 mode: empty cavityF.E.M. simulation


• Microwave moisture meter tests

54

When the cavity is loaded, its resonances undergo a negativefrequency shift f and an increase of the halfwidth g

• these changes (f, g) may be measured with highprecision 0.1 ppm

• a primary method, LoD or cKF, can be used tocalibrate the frequency response of different moistsubstances

antennas mounted on the lateralsurface of the cylindrical resonator

Calibration against a traditional moisture analizer

Moist tobaccoflakes

LoD moistureanalizer

f 2~ 10 MHz f1 ~ 23 MHz

f1f2

Progress in WP2

55

three different types of moistsample holders were designedto match the features anddimensions of both INRiM andCETIAT moisture meters

• INRIM• Design of moisture-tight holders for

sample transport between INRIM and CETIAT (D2.2.4)

Progress in WP2• MIKES: A preliminary test on using a RH/T logger for

monitoring a sample during transportation (D2.2.2)

56

Logg

erin

the

sam

ple

Logg

eron

the

sam

ple

37.5%rh

73.5 %rh


monitoring a sample during transportation (D2.2.2)• Change in RH reading (in both locations):

37.5 %rh 73.5 %rh

• Change in moisture content (determined with LoD): 5.8 %mc 12.6 %mc

• According to [1], the RH change corresponds to 7 %mc, which is in very good agreement with the LoD measurement

[1] K. K. Hansen, Sorption isotherms, Technical Report 162/86, The Technical University of Denmark


monitoring a sample during transportation (D2.2.2)• Limited to low moisture range

• Note also the difference between adsorption and desorption

[1] K. K. Hansen, Sorption isotherms, Technical Report 162/86, The Technical University of Denmark

Progress in WP2• NPL

59

Progress in WP2• UL

60

Progress in WP2• TUBITAK

61

Progress in WP2• UT

62


63

No Description Original Actual Status & Notes2.1.1 The list of candidate materials

prepared May 14 May 14 This deliverable is completed.

2.1.2 Uncertainty analysis data for CRM

Jan 15

2.1.3 At least one new CRM available

Sep 15


64

No Description Original Actual Status & Notes2.2.1 Review report on procedures

relevant to transportation of samples and CRMs

May 14 .

2.2.2 Submission paper on the RH/T logger based sample monitoring method (effect of transportation)

Jul 15

2.2.3 Submission of paper on the effect of ambient conditions and packaging (wooden samples)

Mar 15

2.2.4 At least 3 sample holders designed and tested

Sep 14 Sep 14 The deliverable is completed.

2.2.5 Submission of paper on the effect of ambient conditions and packaging (food and pharmaceutical, paper)

Nov 14

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

Aug 15

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

Sep 15


65

No Description Original Actual Status & Notes2.3.1 Design of resonant or non resonant

coaxial cells for RF/MW transfer standard instrument

May 14 May 14 This deliverable is completed.

2.3.2 At least 4 resonant or non resonant coaxial cells ready

Nov 14

2.3.3 Complete RF/MW transfer system with initial tests

Mar 15

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

Sep 15

2.3.5 Microwave moisture meter Nov 14 Nov 14 The delivery is completed.

2.3.6 Portable humidity generator Mar 14 Nov 14 The delivery is completed.

2.3.7 Complete transfer standard system with initial tests

Sep 15

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

Jan 16

2.3.9 Reference measurements for transfer standards tests

Jan 16


66

No Description Original Actual Status & Notes2.4.1 Design of a calibration system

for sensors measuring surface moisture in polymer elements

May 14 May 14 The deliverable is completed.

2.4.2 Complete system with initial tests

May 15

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

May 14 May 14 This deliverable is completed

2.4.4 Complete system with initial tests

May 15

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

May 15

Highlights in WP3• Model verification for transient heat and mass transfer in non-reactive

porous and partly porous media

• Model verification for water transport in porous materials and associated phase change

• Preliminary measurement uncertainty budgets for different samples compiled by

• UT for the cKF methods,

• INRIM for LoD and cKF methods and

• DTI for LoD+dew point detection method

• Collaborative work to design validation systems for moisture transport in thin polymer layer (UL + REG1) and in bulk materials (INRIM + REG1)

67

68

Outline: WP3 Task 3.2 – Mathematical and numerical model verification

• Model verification for heat and mass transfer in non-reactive porous and partlyporous media (REG D2.1);

• ;

• Model verification for transient heat and mass transfer in non-reactive porousand partly porous media (REG D2.2);

• Model verification for water transport in porous materials and associated phasechange (REG D2.3);

• Model verification for multiscale-modelling of heat conduction (REG D2.4);

69

WP3 – Model verification

The aim was to separately verify the different parts of the mathematical andnumerical models developed within WP3 of the JRP.

A verification procedure has been carried out to test the accuracy and the efficiencyof the proposed Artificial Compressibility (AC) Characteristic Based Split (CBS)algorithm, for the solution of the thermo-fluid-dynamic moisture related problems.

Such an objective has been reached by selecting representative numerical,analytical and experimental benchmarks available in the scientific literature.

VERIFICATION ≠ VALIDATION

Because correct results can be produced also in presence of mathematicalerrors, giving the impression of correctness (right answer for the wrongreason), verification should be performed to a sufficient level before thevalidation activity begins.

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The non-dimensional form of the equations for natural convection problems can bewritten as:Mass conservation equation

Energy conservation equation

Momentum conservation equation

u1

x1

u

2

x2

0

1u1

t

12 u1

u1

x1

12 u2

u1

x2

px1

PrRa

J

2 u1

x12

2 u1

x22

1Da

PrRa

u1

Tt

u1Tx1

u2Tx2

RaPr2 Tx1

2 2 Tx2

2

THE SCALES AND THE PARAMETERS USED TO DERIVE THE ABOVE NON-DIMENSIONALEQUATIONS FOR NATURAL CONVECTION ARE:

3* * * **

* *

*

2

; ; ; Ra ; Pr ; ; ;2

1J ; ; Da ; ; ; ;

h c

f h c fi h cri r

f f f

p peff eff f s f ff f

f f fp pf f

g T T L g L Tx T TT T px T T t t pL T T L g L T

c c uuL c c g L T

Governing equations

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Model verification for heat and mass transfer in non-reactive porous and partly porous media

Natural convection in square porous cavity

Computational domain and boundary conditions

Structured computational grid (3721 nodes, 7200 elements)

Pr=0.71

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Ra=7·104 and Da=10-4 Ra=7·104 and Da=10-3

Ra=106 and Da=10-4 Ra=106 and Da=10-3

The results obtained arecompared with the numericalsolution presented by Basak etal., in terms of dimensionlesstemperature contours.

Reference paper

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Pr=0.71

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Ra=107 and Da=10-4 Ra=105, Da=10-2

Pr=0.71 = 0.4

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Forced convection in horizontal porous cannel


Non-uniform grid with 6400 elements and 3321 nodes


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Forced convection in horizontal porous cannel

1

x

mix i imean x S

T u T dSu S

* The comparison is carried out for the non-dimensional velocity and temperature at a section,where the flow and the thermal field are hydro-dynamically and thermally developed.

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Heat and fluid flow through interfaces between saturatedporous media and free fluids

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Pr=6.97, Ra=3.028·107, Da=7.354·10-7, F=0.6124, ε=0.36, λ=1.397

Pr=6.97, Ra=3.028·107, Da=1.296·10-5, F=0.5647, ε=0.38, λ=1.383

Heat and fluid flow through interfaces between saturatedporous media and free fluids

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Computational domain and boundary conditions employed

Computational grid employed, composed by 40401 nodes and 80000

triangular elements

RaP gKTL / RaDa 102 104 Pr 1

Model verification for transient heat and mass transfer in non-reactive porous and partly porous media

Natural convection in a square buoyancy driven porous cavity

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Temperature contours (left) and streamlines (right) at a real time of 250

(top), 1000 (middle) and 2500 (bottom) for Da=10-8 and Ra=1011

Variation with time of the mean Nusselt number at the hot wall. Comparison with the numerical

solution proposed by Saeid et al., Journal of Heat and Mass Transfer,

2004

Natural convection in a square buoyancy driven porous cavity

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Physical model of transpiration cooling with phase change

Reference paper

J. X. Shi, J. H. Wang, A Numerical Investigation of Transpiration Cooling with

Liquid Coolant Phase Change, Transp Porous Med (2011) 87:703–716

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6 21.0 10Q J m s 0.35 45 10pD m

84



20.5m kg m s0.35 45 10pD m

85



20.5m kg m s 45 10pD m 6 21.0 10Q J m s

86


6 21.0 10Q J m s 20.5m kg m s 0.35


87

Model verification for multiscale-modelling of heat conductionMultiscale-modelling of heat conduction based on the computationalhomogenisation (in which the material response will be obtained from theunderlying microstructure by solving a boundary value problem on arepresentative volume of the microstructure).

88

X

Y

0 0.001 0.002 0.0030

0.001

0.002

0.003

0.004

0.005

0.006

T573.2573572.8572.6572.4572.2572571.8571.6571.4571.2571570.8570.6570.4570.2570569.8569.6569.4569.2569568.8568.6568.4568.2568567.8567.6567.4567.2567566.8566.6566.4566.2566565.8565.6565.4565.2565564.8

Model verification for multiscale-modelling of heat conduction

I. Ozdemir, W. A. M. Brekelmans and M. G. D. Geers. Computational homogenization forheat conduction in heterogeneous solids. International Journal For Numerical Methods InEngineering, 2008; 73:185–204.

Reference paper

Initial study for model uncertainty budgets

Empirical approach to uncertainties identification (Eurachem/CITAC guide on sampling)

89

Process Uncertainty source/class

Type A Type B

Analysis Analytical variability(combined contribution of statistical effects)

Analytical bias(combined effect of bias sources)

Sampling Sampling variability(dominated by heterogeneityand operator variations)

Sampling bias(combined effect of selection bias, operator bias, etc.)

Preliminary model uncertainty budgets

Cause-and-effect diagram for LoD measurements

90

Measuringinstrument

calibrationdrift

Sample

stability

Standard AmbientProcedure

calibration

Operator

sampling temperature

pressure

humidity

parallax

repeatability

buoyancy

vibrations

temperaturematrix

repeatability

end pointstorage

buoyancy

samplepreparation

zeroing

bias

volatiles

bias

Preliminary model uncertainty budgets(e.g. LoD measurements)

91

Symbol Source of uncertainty

±Value(basis for

uncertainty estimation)

Probability distribution Divisor Sensitivity

coefficient

Contribution to combined

uncertainty

Degrees of freedom

IMInstrument measurement effects (incl. mass calibration)

Normal 1 ∞

SC Sample collection and transport

Normal or Lognormal 1 ∞

PM Laboratory preparation method Uniform 3.46

MI Matrix interference (e.g. other volatiles)

Normal or Lognormal 1

SC Sample contamination (e.g. ambient humidity) Uniform 3.46

One row for each input quantity

uc Combined std uncertainty Normal

U Expanded uncertainty Normal (k=2)

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• The following activities will be carried out : Design of experiments for modelling validation; Validation of numerical tools for moisture models; Uncertainty analysis of numerical modelling; Application of the modelling software tool.

The aim is to completely validate the developed numerical code, based on the non-commercial AC-CBS algorithm and finite element approach.Extensive validation of the multi-physics numerical tool developed, whose singlephysics have been verified separately in REG Task 2.

Future activities: Model validation

93

Future activities: model validation

Computational domain

• Free flow;• Porous media flow;• Species transport in porous media.

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ENLARGEMENT

ENLARGEMENT

Computational grid employed


95Qualitative velocity field

Water removal animation



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No Description Original Actual Status & Notes3.1.1 (REG D1.2)

Mathematical modelling of moisture processes in selected materials

Feb 14 Feb 14 Deliverable completed.

3.1.2 Model of temperature distribution

Aug 14

3.1.3 (REG D1.3)

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

May 14 May 14 Deliverable completed.

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

Nov 14

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

Nov 14

3.1.6 Model for diffusion of moisture in paper sheet

Nov 14

3.1.7 Report on model verification May 15


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Report on design of experiments for modelling validation

Jul 15

3.2.2 (REG D3.2)

Report on validation of numerical tools for moisture models

Sep 15

3.2.3 Report on validation of the calibration method for surface moisture

Nov 15

3.2.4 Report on validation of microwave measurement method for bulk moisture

Aug 15

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

Nov 15

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

Aug 15

3.2.7 (REG D3.4)

Report on the application of the modelling software tool

May 16


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Report on uncertainty analysis of numerical modelling

Mar 16

3.3.2 Report on uncertainty evaluations for moisture measurements in paper

Mar 16

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

Mar 16

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