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!!
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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
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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
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REG2: Deliverables
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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
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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?)
WP4: Creating impact – active work
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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?
WP4: Creating impact – active work
15 Are we still targeting these ones?
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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 ☺
WP4: Creating impact – active work
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WP4: Creating impact
Submission deadline 3 July!
Draft some time before that (so make sure M24 details are ready before then).
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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
WP4: Creating impact
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WP4: Creating impact
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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) ?
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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?
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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
WP1: Deliverable in Task 1.2
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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
WP1: Deliverable in Task 1.3
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
Progress in WP2• CETIAT
• Capacitive cell / for solids and for liquids
45mica/silicone
RF electrode
quartz cell
LiquidGround electrode
RF electrode
N connectorTeflon
mica/silicone
Solid samples cell
Progress in WP2• CETIAT
• Capacitive cell / liquid cell results / electrical description
46
Progress in WP2• CETIAT
• Capacitive cell / resonant structure
47
Progress in WP2• CETIAT
• Coaxial cell
48
Samples
Samples
1"5/8coaxial lineSliding short circuit
Progress in WP2• CETIAT
• 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
Progress in WP2• INRIM
• 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
Progress in WP2• INRIM
• 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
Progress in WP2• INRIM
• 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
Progress in WP2• MIKES: A preliminary test on using a RH/T logger for
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
Progress in WP2• MIKES: A preliminary test on using a RH/T logger for
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
WP2: Deliverable in Task 2.1
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
WP2: Deliverable in Task 2.2
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
WP2: Deliverable in Task 2.3
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
WP2: Deliverable in Task 2.4
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.
70
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
71
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
72
Model verification for heat and mass transfer in non-reactive porous and partly porous media
Natural convection in square porous cavity
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
73
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
74
Model verification for heat and mass transfer in non-reactive porous and partly porous media
Natural convection in square porous cavity
Ra=107 and Da=10-4 Ra=105, Da=10-2
Pr=0.71 = 0.4
75
Model verification for heat and mass transfer in non-reactive porous and partly porous media
Natural convection in square porous cavity
76
Forced convection in horizontal porous cannel
Model verification for heat and mass transfer in non-reactive porous and partly porous media
Non-uniform grid with 6400 elements and 3321 nodes
Computational domain and boundary conditions
77
Model verification for heat and mass transfer in non-reactive porous and partly porous media
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.
78
Model verification for heat and mass transfer in non-reactive porous and partly porous media
Computational domain and boundary conditions
Structured computational grid (3721 nodes, 7200 elements)
Heat and fluid flow through interfaces between saturatedporous media and free fluids
79
Model verification for heat and mass transfer in non-reactive porous and partly porous media
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
81
Model verification for transient heat and mass transfer in non-reactive porous and partly porous media
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
82
Model verification for transient heat and mass transfer in non-reactive porous and partly porous media
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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Model verification for transient heat and mass transfer in non-reactive porous and partly porous media
Physical model of transpiration cooling with phase change
6 21.0 10Q J m s 0.35 45 10pD m
84
Model verification for transient heat and mass transfer in non-reactive porous and partly porous media
Physical model of transpiration cooling with phase change
20.5m kg m s0.35 45 10pD m
85
Model verification for transient heat and mass transfer in non-reactive porous and partly porous media
Physical model of transpiration cooling with phase change
20.5m kg m s 45 10pD m 6 21.0 10Q J m s
86
Model verification for transient heat and mass transfer in non-reactive porous and partly porous media
6 21.0 10Q J m s 20.5m kg m s 0.35
Physical model of transpiration cooling with phase change
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.
94
ENLARGEMENT
ENLARGEMENT
Computational grid employed
Future activities: model validation
95Qualitative velocity field
Water removal animation
Future activities: model validation
WP3: Deliverable in Task 3.1
96
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
WP3: Deliverable in Task 3.2
97
No Description Original Actual Status & Notes3.2.1 (REG D3.1)
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
WP3: Deliverable in Task 3.3
98
No Description Original Actual Status & Notes3.3.1 (REG D3.3)
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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