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CIPM 2007-09 (Part 2)

Evolving Needs for Metrology in Material Property Measurements Report of the CIPM ad hoc Working Group on Materials Metrology (WGMM) Part 2: draft Annexes October 2007

Evolving Need for

Metrology in

Material Property

Measurements

Report of the CIPM

ad hoc Working Group

on Materials Metrology

(WGMM) Part 2: draft Annexes

October 2007

1

ANNEX A - VIM 2007 Definitions

2.27 (3.9)

measurement uncertainty

uncertainty of measurement

uncertainty

parameter characterising the dispersion of the quantity values being attributed to a measurand,

based on the information used.

NOTES

1. Measurement uncertainty includes components arising from systematic effects, such as components

associated with corrections and the assigned quantity values of measurement standards, as well as the

definitional uncertainty. Sometimes known systematic effects are not corrected for but are instead treated as

uncertainty components.

2. The parameter may be, for example, a standard deviation called standard measurement uncertainty

(or a specified multiple of it), or the half-width of an interval, having a stated coverage probability.

3. Measurement uncertainty comprises, in general, many components. Some of these may be evaluated

by Type A evaluation of measurement uncertainty from the statistical distribution of the quantity values from

series of measurements and can be characterised by experimental standard deviations. The other components,

which may be evaluated by Type B evaluation of measurement uncertainty, can also be characterised by

standard deviations, evaluated from probability density functions based on experience or other information.

2

2.39

calibration

operation that, under specified conditions, in a first step establishes a relation between the

quantity values with measurement uncertainties provided by measurement standards and

corresponding indications with associated measurement uncertainties and, in a second step,

uses this information to establish a relation for obtaining a measurement result from an

indication.

NOTES

1. A calibration may be expressed by a statement, calibration function, calibration diagram, calibration

cure, or calibration table. In some cases it may consist of an additive or multiplicative correction of the

indication with associated uncertainty.

2. Calibration should not be confused with adjustment of a measuring system, often mistakenly called

‘self-calibration’, nor with verification of calibration.

3. Sometimes the first step alone in the above definition is perceived as being calibration.

2.41 (6.10)

metrological traceability

property of a measurement result whereby the result can be related to a stated reference through a

documented unbroken chain of calibrations, each contributing to the measurement uncertainty.

NOTES

1. For this definition, a ‘stated reference’ can be a definition of a measurement unit through its practical

realisation, or a measurement procedure including the measurement unit for a non-ordinal quantity, or a

measurement standard.

2. Metrological traceability requires an established calibration hierarchy.

3. Specification of the stated reference must include the time at which this reference was used, along

with any other relevant metrological information about the reference, such as when the first calibration in the

calibration hierarchy was performed.

4. For measurements with more than one input quantity in the measurement model, each of the input

quantities should itself be metrologically traceable and the calibration hierarchy involved may form a

branched structure or a network. The effort involved in establishing metrological traceability for each input

quantity should be commensurate with its relative contribution to the measurement result. 5. Metrological traceability by itself does not ensure adequate measurement uncertainty or absence of

mistakes. 6. A comparison between two measurement standards may be viewed as a calibration if the comparison

is used to check and, if necessary, correct the quantity value and measurement uncertainty attributed to one of

the measurement standards.

7. The abbreviated term “traceability” is sometimes used for ‘metrological traceability’ as well as for

other concepts, such as ‘sample traceability’ or ‘document traceability’ or ‘instrument traceability’, where the

history (‘trace’) of an item is meant. Therefore, the full term is preferred.

3

2.42

metrological traceability chain

traceability chain

sequence of measurement standards and calibrations that is used to relate a measurement

result to a stated reference

NOTES

1. A metrological traceability chain is defined through a calibration hierarchy.

2. The metrological traceability chain is used to establish metrological traceability of the measurement

result.

3. A comparison between two measurement standards may be viewed as a calibration if the comparison

is used to check and, if necessary, correct the quantity value and measurement uncertainty attributed to one of

the measurement standards.

2.43

metrological traceability to a measurement unit

metrological traceability to a unit

metrological traceability where the stated reference is the definition of a measurement

unit through its practical realisation

NOTE

The expression ‘traceability to the SI’ means metrological traceability to a measurement unit of the

International System of Units.

2.46

metrological comparability of measurement results

metrological comparability

comparability of measurement results that are metrologically traceable to the same

reference

EXAMPLE

Measurement results, for the distances from Earth to Moon and from Paris to London, are

comparable when they are both metrologically traceable to the same measurement unit, for

instance the metre.

NOTES

1 — See Note 1 to 2.41 metrological traceability.

2 — Metrological comparability of measurement results does not necessitate that the measured quantity

values and associated measurement uncertainties compared are of the same order of magnitude.

4

ANNEX B TASK GROUP 1 – MECHANICAL PROPERTIES

Table B1a Modulus measurement

Modulus Scope Determination of the stiffness in the elastic or visco-elastic range of response under tensile

deformation.

Material Category Metal, ceramic, polymer, composite, rubber, biomaterials

Material State and

Scale

Bulk, micro, film, nano, surface.

Regulation Need FIA Technical Regulations, nuclear industry material specifications; structural integrity,

fracture mechanics and design codes. ASME boiler & pressure vessel codes

User needs Reliable data for FE modelling and stiffness controlled design, material specifications,

measurements on novel materials (e.g. MMCs) and the variation with temperature.

Accreditation needs Yes, Formula One Technical Relegations

Comparability Yes, as above “some teams faced potential disqualification as results that were acceptable in

the in-house testing were actually exceeding the 40 limit when tested independently”.

Need for

intercomparison

Yes

Economic impact

studies

No

Number of existing

methods

Many existing standards (ISO, ASTM) cover different materials and test methods.

The European TENSTAND project has developed a preferred procedure for tensile testing.

Standardisation

situation

ASTM E111 is the only standard specifically for measuring the Young's modulus of metals

from the tensile test. EN 10002 does not mention modulus at all. Dynamic methods (ASTM

E1875 and E1876) designed for use with ceramics.

NMI/MRI activities NPL.

R & D phase? Yes, certification of a modulus reference material, development of dynamic methods.

Traceability issues Modulus traceable to mass and length

SI units relevant Length (strain), mass (force)

CCs coverage No

Prior studies (method

specific)

TWA20 and NPL activity on modulus of MMCs VAMAS TWA20 Report Validation of a

Draft Tensile Testing Standard for Discontinuously Reinforced MMC. B. Roebuck, J.D.

Lord and L.N. McCartney, May 1995B. Roebuck, J.D. Lord, P.M. Cooper and L.N.

McCartney. Data Acquisition and Analysis of Tensile Properties for Metal Matrix

Composites, ASTM J. Testing and Evaluation, JTEVA, 22(1), 1994, 63-69.TENSTAND

activity - generation and analysis of tensile ASCII datafiles, modulus study and

recommendations for future developments. TENSTAND WP2 Report – Digital Tensile

Software Evaluation. J D Lord, M S Loveday, M Rides, I McEnteggart. July 2004.

TENSTAND WP3 Report – Modulus Measurement Methods. J D Lord, M Rides, M S

Loveday. January 2005

Method comparability Some data has been generated from intercomparison exercises (TWA20 example attached).

Limited data on comparison with dynamic methods, or measurements at temperature.

No validated modulus reference materials.

Yes - universal tensile testing equipment, but requirements might include specialised

alignment cells and averaging strain measurement. Dynamic test equipment is less widely

available.

Standard test machines

Different machines have not been directly compared using a reference material and agreed

test method.

Calibration – reference

materials

No - a BCR tensile reference material is available, but it has not specifically been certified

for modulus measurement

5

Table B1b Modulus measurement

Modulus Issue / Evidence Comment / Plan

Material Property Modulus values are the normal starting point

for finite element analysis (FEA) that is used to

analyse the distortion and load carrying

capacity in most structural applications. Can

be a controlled parameter (e.g. specific stiffness

limit on materials that can be used in Formula

1).

Is the material property

important?

Round-robins and industrial experience (e.g.

Formula 1) demonstrate repeatably that

modulus measurements are unsatisfactory. Also

shown by round - robin data (see Figure 2).

Is there a problem with

consistency /

comparability of the

measured material

property?

Basic measurements of force (mass) and strain

(= displacement = length) should be

satisfactory. There can be differences in how

the displacement is measured, such as gauge

length used, sensor type used (e.g. clip gauge,

strain gauge, digital image correlation) and the

data analysis procedures used.

Is the problem caused

by an unaddressed need

for traceability?

Alignment is important for both the loading

machine and specimen.

What other aspects are

relevant to the problem?

Errors in analysis due to incorrect modulus

values could have serious and costly failures.

In the particular case of Formula 1, the

financial penalty of disqualification could be

extremely high and threaten the viability of the

company (e.g. Williams Grand Prix annual

expenditure is £100m).

Are there important

consequences if this

problem is not

addressed?

Modulus measurement relies on two CCs (i.e.

CCM and CCL) for traceable measurements,

who would not normally have a combined

study. A detailed study of the strain

measurement methods available and the data

analysis is needed. Both these aspects would

be suitable for CIPM and ILAC involvement.

A proposal has been made (see Annex A) to

undertake a RR in order to extend an existing

creep testing approved reference material to

modulus as well.

What is the way

forward?

Undertake a round-robin based on using the

BCR Nimonic 75 reference material, which is

certified for creep measurements but not for

modulus measurements.

6

Table B2a Hardness measurement

Nano-Indentation

Scope Mechanical properties of nano-size thin film, hardness, modulus, strain-

load, and adhesion strength. Hardness expressed in penetration depth or

indent size

Material Category Mostly Metal, ceramic, polymer, composite, thin film covered on base

materials

Material State and Scale Solid, bulk, film, nano, surface.

Regulation Need Yes, ISO 14577

User needs Material producer, semiconductor designer and fabricator, and end users.

There are strong needs from those industries. Especially for quality

control of heat treated material

Accreditation needs Yes

Compatibility Yes. Especially, strict test condition is required to provide more reliable

equivalency of test results

Need for intercomparison Intercomparison should be conducted. WGH is currently carrying

intercomparison for conventional hardness such as Rockwell, Vickers,

Brinell

Economic impact studies None. No. However, most of the NMIs are working together through

activities of WGH to reduce the scattering of data.

Number of existing methods At least three major methods for conventional hardness measurement.

There are many other test methods.

Standardization situation "Thin film" of TWA22, VAMAS Hardness (Nano-Indentation):

Standardization activities are under discussion at TWA22 of VAMAS.

ISO 6508, 6507, 6506, etc. including 14588 for Nano indentation..

NMI/MRI activities UK NPL, KRISS, MRI=Professor Takai of Nagoya University and NIMS

have studied.

R & D phase ? Yes, especially for the effect of indenter geometry on the measurement

and nano-hardness measurement. There are many basic research

activities in this field. Especially, nano-indentation researches under

various circumstances are active.

Traceability issues WGH under CCM is working to provide internationally agreed standard

reference value for the traceability issue. Comparability is an issue in

hardness. Accuracy of loading, displacement and in some cases

temperature measurements, record of temperature of specimen

throughout a test, measurement of dimension of scratch on specimen.

SI units relevant Temperature, length, stress, and time. (Unique unit such as HRC, HRB,

HV, etc. Not traceable back to SI unit directly).

CCs coverage (same as the above SI units)

Prior studies (method specific) TWA22 of VAMAS

Method comparability Still under discussion.

Standard test machines None.

Some reference materials are sold in the market. But there are no publicly

standardized references.

Calibration - reference

materials

CRM (DLC on steel) with certified critical failure loads under scratch test

(BCR-692); CRM with certified indentation stiffness under development

at NPL (ref. Nigel Jennett)

Comments Hardness (Nano-Indentation): Standardization activities are under

discussion at TWA22 of VAMAS. Although testing procedures are

standardized as ISO14577, there are still remaining discussions at ISO..

7

Table B2b Hardness measurement

Hardness Issue / Evidence Comment / Plan

Material Property Controlled property in many cases,

such as bolts

Property measurements are

very procedure-related (e.g.

Vickers, Brinell)


important?

Consistency is controlled through

reference blocks - normally steel

EU and VAMAS is studying

microinjection and developing

reference materials.


consistency / comparability of

the measured material property?

Scatter is acceptable

Is the problem caused by an

unaddressed need for

traceability?

Trend now to derive conventional

properties (e.g. modulus, strength)

from these measurements, especially

at micro-scale.

Work on micro-hardness is

more likely to be undertaken in

materials area than in Mass

groups.

What other aspects are relevant

to the problem?

The production of many industrial

goods from tool steels to bolts are

dependent almost solely on hardness

values that are dependent on material

transfer standards.

Are there important

consequences if this problem is

not addressed?

Hardness is probably one of the most

procedure dominated material

properties. It is also one of the most

frequently quoted.

Hardness could easily be

treated outside CCM as it does

not meet the scope of SI related

work, but is more akin to other

material property

measurement.

What is the way forward?

8

Table B3a Toughness

Toughness Scope Measurement of Mode I, II or mixed mode fracture toughness

Material Category Metal, ceramic, polymer, composite

Material State and Scale Bulk, film

Regulation Need ASME 10?

User needs To have confidence that the data used to design structures such as

pressure vessels that are safety critical are reliable.

Accreditation needs Checking pressure vessel codes

Comparability Yes, designs must be reliable regardless of source of data

Need for intercomparison Take advice from IRMM based on their current work

Economic impact studies Safety critical applications have major consequenes when failures

occur.

Number of existing methods Mode 1 standards well established, Mode II being developed,

Standardisation situation Many standards exist for metals, composites (ISO 15024), polymers

NMI/MRI activities IRMM running RR (NIST, IRMM, AIST, LNE)

R & D phase? Continuation, effect of different methods on measurand, adapting

procedures at ISO TC164 level C18

Traceability issues Fracture toughness is a critical property for safety analysis of structures

SI units relevant mass (kg), time (s),

CCs coverage No

Prior studies (method specific) Precision data given for ISO 15024

Method comparability Yes, Comparison of different Mode II tests for composites in VAMAS

USA/Japan reference machines Standard test machines


materials

Master batch CRM approach

9

Table B3b Toughness

Toughness Issue / Evidence Comment / Plan

Material Property Toughness data are normally used at a

later stage of product design to assess

component toughness and that

minimum values are obtained. This

particular important for applications,

such as, pressure vessels (see ASME

and CEN Standards)

Is the material property important? Currently, IRMM round-robin

underway aimed at comparing

procedures (e.g. ASTM vs. ISO).

Is there a problem with consistency

/ comparability of the measured

material property?

Basic measurements of force (mass),

strain (= displacement = length) and

time (second) should be satisfactory.


unaddressed need for traceability?

Quality and consistency of any pre-

cracking is important

What other aspects are relevant to

the problem?

Potentially severe consequence if

failure occurs as toughness values

have high uncertainty (e.g. pressure

vessels)

Are there important consequences if

this problem is not addressed?

Toughness measurement relies on

three CCs (i.e. CCM, CCL and

CCTF) for traceable measurements,

who would not normally have a

combined study. Propose to assess

IRMM study for the presence and

impact of any "metrology" aspects

that would be suitable for CIPM and

ILAC involvement.

What is the way forward? Evaluate other exercises, such as run

by IRMM to determine if further

work is justified.

10

Table B4a Ultimate Strength

Strength Scope Ultimate strength, or in some systems - yield strength

Material Category Metal, ceramic, polymer, composite, rubber, etc.?

Material State and Scale Bulk, micro, film,

Regulation Need ISO 898 Mechanical Properties of Fasteners - Part 1. Bolts, screws and studs

specifies heat bolts etc. shall have the properties specified in Table 3 [using

ISO 6892 - tensile strength (n/mx), lower yield stress (n/mx), proof stress

((n/mx), impact strength (mi), Brinell, Rockwell and surface hardness,

elongation after fracture]. Property lists are also shown for -20, 100, 200, 250

and 300C, although not part of the standard.

User needs Minimum (mi), nominal (n) or maximum (mx) values..

Accreditation needs ISO 898 and any document calling up ISO 898, such as Eurocode 1993-1-8,

Also BS 4882

Comparability Yes

Need for intercomparison Yes

Economic impact studies

Number of existing methods Many to be entered for all materials (e.g. ISO 527 for composites), Note no

common material independent method.

Standardisation situation

NMI/MRI activities

R & D phase? Biaxial strength measurement in VAMAS, Japan planned research on end-tab

design

Traceability issues Traceability via SI units and accredited test machines

SI units relevant Length (dimensions), mass (force)

CCs coverage No


specific)

Method comparability

No Standard test machines

No


materials

BCR material (see modulus)

Table B4b To be added

11

Table B5a Creep

Creep Scope Creep is a gradual change behaviour in shape under stress, and it is pronounced

especially at the elevated temperatures over about one third of the melting point in

absolute temperature. Generally, uniaxial tensile stress condition is used similar to

tensile test, and a deformation of gauge portion of a cylindrical specimen is measured

with time at a constant temperature, therefore, temperature of a specimen should be

also measured as well as deformation.

Material Category Metal, ceramic, polymer, and composite, etc, however, metallic materials are in highest

demand.

Especially, high temperature resistant metals that may be tested under 600 to 700

degree C and superalloy materials that may be tested under 1000 degree C or over are

the hottest issues.

Material State and

Scale

Bulk material for power engineering, engine, and petrochemical plant, and nanoscale

wire used in LSI.

Regulation Need Regulated in JIS, ISO, ASTM, etc.

Major regulations and standards are:

ISO 204:1997 Load: ±0.5%(Class 0.5), ±1.0%(Class 1), ±2.0%(Class 2)

Temperature: ±3oC (T � 900

oC), ±4

oC (900

oC < T � 1000

oC)

ASTM E139-96:1996 Temperature: ±3oF (T �1,800

oF), ±5

oF (1,800

oF < T)

JIS Z2271:1999 Load: ±0.5% (Creep test), ±1.0% (Creep rupture test)

Temperature: ±3oC (T �900

oC), ±4

oC (900

oC < T � 1,000

oC)

User needs Material producer, plant designer and fabricator, and end user of plant. LSI designer

and manufacturer.

There are several tens of companies, mainly steel, heavy, power-generation,

petrochemical plant industries, which have creep test equipments. There are more than

ten organizations which implement creep tests and provide data as a business. NIMS id

one of these testing organizations.

Accreditation needs Yes. Screening of data with its quality is required prior to evaluation. These needs are

not required by regulatory laws, but accuracy of load, temperature, displacement is

strictly required by various standards.

Compatibility Yes. Because It is impossible to obtain full set of creep data in one organization.

But, there exist no schemes to ensure comparability of creep test data. Data varies

testing organization by organization.

Need for

intercomparison

Intercomparison should be conducted.

But, even among domestic community, lack of data accuracy and comparability is

always argued.

Economic impact

studies

Yes, it has been conducted, however, it is insufficient.

1) Example of too big safety margins

Economic loss due to accidents and defects of industrial products is estimated as big as

4% of GDP. (Refer to the report, Takanobu Murakami, "Huge accidents and current

science and technology", NSK Technical Journal, No.675 (2003)�Prevention of those

accidents is important not only to secure safety of people, but also to support economic

growth. Major reasons of those accidents are generally defined as a result of

insufficient quality in fatigue, corrosion and abrasion, and creep of materials. For those

high temperature structural parts, which are used for power-generation plants,

petrochemical plants, and jet planes and automobiles, creep defects are one of major

reasons of material degradation.

For example, 81% of power-generation boilers failures are due to mechanical

destruction of boiler materials, and among those 81% of accidents, creep fracture is the

major reason. In order to design safe power-generation plants, long term creep strength

data are mandatory. In the case where no accurate creep data are provided, safety

margin is necessary and plants are to be operated at lower vapour temperature to

prevent creep degradation of boiler materials. Lower vapour temperature causes lower

generation efficiency. 20� change of vapour temperature causes 1% loss of generation

efficiency, and this means that 2,580,000kl of fuel (Heavy oil equivalent) is lost in

Japan annually. If accurate creep test data could be available and 1% increase in

efficiency could be obtained, 70,000,000,000 yen could have been saved, and

9,430,000tons of CO2 could have been reduced.

12

Economic impact

studies

Talking about recent power-generation plants in Japan, cost savings of approximately

100,000,000yen per day can be obtained based on creep test data acquisition and data

based design compared to plants operation of 20 to 30 years ago. However, death and

injury accidents such as accidents at Mihama Nuclear Power Plant and Hamaoka

Nuclear Power Plant due to creep fracture of pipes result in huge loss in human lives

and repair costs; and alternate plant construction and operation.

Number of existing

methods

There are several codes and standards for creep test, however, the contents are

essentially the same each other. For example, ISO 204:1997, ASTM E139-96:1996,

JIS Z2271:1999

Standardization

situation

NIMS Creep Data Sheets are the greatest precision creep data sources.

European Creep Collaborative Committee (ECCC) has summarized and has reported

"ECCC Recommendations" in 2001.

NMI/MRI activities NMI=No.

MRI=NIMS: Acquisition of creep property data for various materials, and those data

are open via internet homepage and NIMS Creep Data Sheets to the public. NIMS

Creep Data Sheets are the greatest precision creep data sources.

http://mits.nims.go.j

R & D phase? Yes, there are many basic research projects on creep properties, however new

measurement techniques are less studied.

Therefore, creep tests are in actually applied stage as a whole, but still R&D activities

are needed.

Traceability issues Accuracy of loading, displacement and temperature measurements, record of

temperature of specimen throughout a creep test, measurement of dimension of

specimen and calibration of thermocouples prior and after creep test.

SI units relevant Temperature, length, stress, and time.

CCs coverage Temperature=CCT, length=CCL, stress=CCM, and time=CCTF. However, creep

properties of materials are mixture of these areas, and systematic coverage for creep

properties of materials are not enough.


specific)

There are many studied have been conducted. The first creep test in continental Europe

area started nearly one century ago in Czech republic.

Recently, creep tests under higher temperature, more than 1000 degree C, are

investigated and some round robin tests are conducted in Japan.

Method comparability Although standardized test methods are completed, data for the same test specimens

vary, and international, even national, comparisons are impossible.

Influence of fluctuation in temperature and load, and dimension of specimen affect on

comparability and studies on these elements have been conducted.

Standard test

machines

There are many creep test machines and measuring devices, appropriate to the codes

and standards.

For example, ISO 204:1997, ASTM E139-96:1996, and JIS Z2271:1999.

Yes there were. However, it may be not at present. Calibration -

reference materials

BCR-425 (Nimonic with certified creep rate at 400 oC, time to 2 % strain, time to 4 %

strain, certified by IRMM, collaboration with NPL)

Comments Testing procedures have been already standardized. In reality, in order to get a set of

creep test data, several institutes must collaborate each other because creep test needs

very long term. Those collaboration tests sometimes cause discussion about

comparability of data among test results derived by different institutes. WGMM should

focus on conventional properties that have comparability problems. Leading edge

properties such as Nano-scale properties may be focused on because of its boom, but

these properties should be discussed and standardized by VAMAS or ISO first and it is

not the time to discuss at WGMM at this moment.

13

Table B5b Creep

Creep Issue / Evidence Comment / Plan

Material Property For example, 81% of power-generation boilers are

due to mechanical destruction of boiler materials, and

among those 81% of accidents, creep fracture is the

major reason. In order to design safe power-

generation plants, long term creep strength data are

mandatory. In the case where no accurate creep data

are provided, safety margin is necessary and plants are

to be operated at lower vapour temperature to prevent

creep degradation of boiler materials. Lower vapour

temperature causes lower generation efficiency. 20�

change of vapour temperature causes 1% loss of

generation efficiency, and this means that 2,580,000kl

of fuel (Heavy oil equivalent) is lost in Japan

annually. If accurate creep test data could be available

and 1% increase in efficiency could be obtained,

70,000,000,000 yen could have been saved, and

9,430,000tons of CO2 could have been reduced.


important?

Although standardized test methods are completed,

data for the same test specimens vary, and

international, even national, comparisons are

impossible.

Influence of fluctuation in temperature and load, and

dimension of specimen affect on comparability and

studies on these elements have been conducted.


consistency / comparability

of the measured material

property?

Although standardized test methods are completed,

data for the same test specimens vary, and

international, even national, comparisons are

impossible.

Influence of fluctuation in temperature and load, and

dimension of specimen affect on comparability and

studies on these elements have been conducted.



traceability?

Temperature=CCT, length=CCL, stress=CCM, and

time=CCTF. However, creep properties of materials

are mixture of these areas, and systematic coverage

for creep properties of materials are not enough.



Are there important

consequences if this problem

is not addressed?


14

Table B6a Fatigue properties

Gigacycle fatigue Scope Ultrasonic fatigue testing to evaluate fatigue properties beyond 10^7 cycles into

gigacycle regions.

Material Category Metal (steel, super alloy, titanium, aluminium, magnesium alloy)

Material State and Scale Bulk material.

Regulation Need None.

Gigacycle fatigue property is rather new methods and conventional evaluation

methods cannot be applied.

User needs Major steel makers, car makers, heavy industries, etc in Japan purchased the

ultrasonic fatigue testing machines in recent 2 or 3 years. They wish it to be a

standard.

Accreditation needs No.

Gigacycle fatigue test methods are under development.

Compatibility None.

Even comparison among different institutions has not been studied.

Need for intercomparison We are investigating the validity and limitation of these test methods, but this must

be done with many other institutes in the world.

Economic impact studies None.

Gigacycle fatigue property is rather new methods and conventional evaluation

methods cannot be applied. In the fields of gigacycle fatigue property, due to lack

of information and data, parts must be made with bigger safety margin and

relatively big economic impacts exist.

Number of existing methods None.

Standardization situation None.

Research works are under development.

NMI/MRI activities NMI=None.

NRI=NIMS has been one of the major research institutions in this field.

R & D phase? The ultrasonic fatigue testing machine is already on the market, but basic research

is still required to assure the validity and limitation.

Traceability issues The ultrasonic fatigue-testing machine is generally calibrated by measuring the

displacement at an edge of a specimen, and temperature of specimen during the test

or the pre-test must be checked. Regulations and standards are required for these

procedures.

SI units relevant Stress (MPa), length (mm), Frequency (kHz)

CCs coverage (same as the above SI units)

Prior studies (method specific) Studies for the ultrasonic fatigue testing began in 1950s and came to a peak in

1980s. Although the studies once declined in 1990s, they were stimulated again in

this century since several institutes (our institute) succeeded in demonstrating the

validity of the ultrasonic fatigue testing on several conditions.

Papers:

Method comparability None.

Standard test machines None.

Calibration - reference materials None.

Comments Traditional fatigue testing procedures are specified by various standards. NIMS do

not think that WGMM would better taking this issue as current issue to be

discussed. Among various methods for testing fatigue properties, Giga-cycle

fatigue test that extends more than 10E+07 cycles and new testing procedures are

under development could be an issue at WGMM.


15

Table B7a Impact properties

Charpy impact test

Scope Resistance of structural steels to pendulum impact load; future: also

used more for checking quality of dispersion of strengthening phase

in brittle matrix (e.g. carbon nanotube in polymer)

Material Category steel, composites

Material State and Scale bulk, macroscopic

Regulation Need existing EU directive on Pressure Equipment

User needs global harmonisation of machine verification needs

Accreditation needs uncertainty budget (new documents at DIS stage in ISO)

Compatibility 2 different hammer tup (2 mm vs 8 mm radius)

Need for intercomparison currently organised between NIST, LNE, NMIJ and IRMM

Economic impact studies No recent studies available to the author's knowledge

Number of existing methods 2

Standardization situation ASTM E23: 8 mm, ISO-148 : now 2 and 8 mm, no more specific JIS

or EN

NMI/MRI activities NMIJ, LNE, IRMM, BAM, NIST

R & D phase? not active

Traceability issues ASTM: to NIST pendulums, ISO: to results obtained in accordance

with documentary standard

SI units relevant kg, m, s

CCs coverage CCM, CCL, CCT

Prior studies (method specific) intercomparisons 1999, 2004

Method comparability material-dependent difference between 2 mm and 8 mm method

Standard test machines 8 mm: NIST pendulums (defined in ASTM standard), 2 mm/8 mm:

reference machines defined by performance criteria in ISO

Calibration - reference

materials

CRMs from NIST, LNE, NMIJ, IRMM

Comments See also strength return - bolts standard - ISO 898


16

Table B8a Rheological properties - viscosity

Viscosity Scope Rheological properties (& surface tension)

Material

Category

Polymers, polymer solutions, composites, rubbers, metals, ceramics

State and Scale Liquid, particle

Regulation Need Gas Industry Standard GIS/LC12: 200611 specification for sealant systems for joint repair on

metallic distribution systems operating at pressures equal to or less than 2 bar, buried in

locations subjected to low traffic loads.

User needs Viscosity when tested in accordance with Annex A shall not be less than 2 centistokes or

greater than 5 centistokes at 25C. Also a surface tension requirement between 25 and 30

mN/m at 25C.

Accreditation

needs

Comparability Yes, a multitude of methods exist for measuring rheological properties (other than Newtonian

viscosity) that do not necessarily produce the same values dependant on the deformation

history

Need for

intercomparison

Low viscosity Newtonian fluids at low deformation rates probably adequately covered. Need

for intercomparisons of Newtonian viscosities at higher values and rates, and non-Newtonian

viscous and viscoelastic behaviour.

Economic impact

studies

Number of

existing methods

Usually glass capillary viscometers (e.g. Ubbelohde capillary viscometers) used to measure

viscosity /reference fluids - restricted to low viscosity Newtonian fluids

Standardisation

situation

ISO 3104 Petroleum products -- Transparent and opaque liquids -- Determination of

kinematic viscosity and calculation of dynamic viscosity

ISO 3105 Glass capillary kinematic viscometers -- Specifications and operating instructions

ASTM D2162-06 Standard Practice for Basic Calibration of Master Viscometers and

Viscosity Oil Standards

For additional ISO standards see below. Many of these techniques are industry sector specific

and not expected to produce comparable values due to the method, but some purport to

determine true viscosity values.

NMI/MRI

activities

e.g. PTB, Germany for Newtonian reference fluids

R & D phase? Established reference fluids. High viscosity fluids and non-newtonian fluids NOT adequately

covered.

Traceability

issues

Through SI units, implemented through reference fluids

SI units relevant Length, mass (stress), time, temperature

CCs coverage Yes - for Newtonian viscosity (under Mass)

CCM.V-K1.A Viscosity measurements of standard liquids 2002,

CCM.V-K1.B1 Viscosity measurements of standard liquids 2002,



CCM.V-K1.C Viscosity measurements of standard liquids 2002,

COOMET.M.V-K1 Viscosity measurements of standard liquids 2005 - 2006, In progress

Prior studies

(method specific)

For high viscosity non-Newtonian fluid properties, several interlaboratory studies undertaken.

Method

comparability

Yes, for Newtonian fluids

Yes - for Newtonian fluids Standard test

machines Yes - for Newtonian fluids

Calibration –

reference

materials

Yes, e.g. as issued by PTB, Germany. These are relatively low in viscosity (0.001 Pa.s to 700

Pa.s) and are for Newtonian viscous behaviour only. The relative uncertainty of the viscosity

for reference liquids provided by the Physikalisch-Technische Bundesanstalt is from 0.2% up

to 1.0% of their value.

17


18

ANNEX C TASK GROUP 2 – THERMAL PHYSICAL PROPERTIES

Table C1a To be added

Table C1b Thermal Conductivity

Thermal Conductivity Issue / Evidence Comment / Plan

Material Category - Thermal insulation, refractory materials,

metal, ceramic, glass, polymer, composite,

Material State and Scale - Foam, Blanket, Bulk, coating, thin

plate, ( +film)

Material Property Regulation Need - Council Directive 93/76/EEC of 13

September 1993 to limit carbon dioxide emissions by

improving energy efficiency (SAVE)

User needs - Customers for conductivity measurements: cars

manufacturers, airplane industry, nuclear industry, defence,

polymers, isolating building structures sectors, etc. Demands

are related to measurements (for establishment of predictive

models, for characterization) and to calibration of

instruments.

Accreditation needs - Accredited testing laboratories for

thermal conductivity measurement need traceability

Customers for

conductivity

measurements: cars

manufacturers, airplane

industry, nuclear industry,

Ministry of Defence,

polymers, isolating

building structures sectors,

etc. Demands are related

to measurements (for

establishment of

predictive models, for

characterisation) and to

calibration of instruments.


important?

ISO (x4) standards, ASTM (x4) standards, CEN standards

have been established.

NMI/MRI activities

NIM(China),

LNE(France),

PTB(Germany),

IPQ(Portugal),

VNIIM(Russia),

NPL(UK), NIST(USA),

JTCCM(Japan)


consistency /


measured material

property?

Traceability is well established for low conductivities, where

reference materials exist. For medium to high conductivities,

a demand of reference materials was identified, but few are

available on the market. A need is especially expressed for

the characterisation of ceramics and new polymers.

Manufacturers of instruments are also requiring reference

materials for the calibration of their instruments. For classic

materials, no specific problem of metrological traceability

was identified. Reference methods exist (available at NMIs),

but a lack of reference materials was observed.

Nevertheless, for new materials linked to micro and nano

scale, a real traceability problem has been identified.

Emergent sectors (electronic and bio) have expressed their

needs for conductivity measurements.

Is the problem caused by

an unaddressed need for

traceability?

Standardization situation - ISO (x4), ASTM (x4) and CEN

standards have been established.



Are there important


problem is not

addressed?

Thermophysical properties are covered by CCT WG9

“Thermophysical property”.

.

What is the way

forward?

Pilot comparison of thermal conductivity of insulation by the

guarded hot plate method is under progress by CCT WG9

19


Table C2b Thermal Diffusivity

Thermal

diffusivity

Issue / Evidence Comment / Plan

Thermal diffusivity

above room

temperature

Material Category

Metal, ceramic, semiconductor, carbon, glass, polymer,

composite,

Material State and Scale

Bulk, coating, thin plate, ( +film)

Is the material

property

important?

Regulation Need

No

User needs

Basic information for thermal design. Production control in

metallurgy and ceramic industries

Accreditation needs

Accredited testing laboratories for thermal diffusivity

measurement need traceability

For example, gas turbine

used for electric power

plants and airplanes need

traceable und comparable

thermal diffusivity values of

turbine blade materials and

coatings.

Is there a problem

with consistency /

comparability of

the measured

material property?

Number of existing methods - There are a few papers, which

compare thermal diffusivity measured by laser flash method

and calculated from thermal conductivity measured by steady

method and heat capacity by differential scanning

calorimeter.

7 standards have been issued for the laser flash method.

NMI/MRI activities

NIM(China), LNE(France),

KRISS(Korea), NPL(UK),

NMIJ(Japan)

Is the problem

caused by an

unaddressed need

for traceability?

The laser flash method has been well established. A few round robin

measurements were

performed among research

institutes using laser flash

method. NMIs did not

participated in these and the

measurements were not SI

traceable.

What other aspects

are relevant to the

problem?

In order to measure thermal diffusivity of thin films, the ultra

fast laser flash method has been developed by picosecond and

nanosecond thermoreflectance technique.

Supply of certified reference material is the traceability rote

for thermal diffusivity.

Calibration – reference materials

Isotropic graphite (NMIJ, Japan), Alumina, Pure iron, Inconel

600, 310 Stainless steel, Nimonic 75 (NPL, UK), BCR-724

(IRMM)

Uncertainty budgets have been developed for these

measurements by NMIJ, Japan, and LNE, France.

Are there

important

consequences if

this problem is not

addressed?

What is the way

forward?

Thermophysical properties are covered by CCT WG9

“Thermophysical property”

Pilot comparison of thermal

diffusivity by the laser flash

method is under progress by

CCT WG9.

20


Table C3b Thermal Expansion

Thermal expansion Issue / Evidence Comment / Plan

Material Category

Metal, ceramic, semiconductor, carbon, glass, polymer

Material State and Scale - Bulk, film


important?

Regulation Need - No

User needs - Basic information to evaluate

deformation of products and thermal stress dependent

of temperature. thermal shock resistance.

Accreditation needs - Accredited testing laboratories

for thermal expansivity measurement need traceability


consistency /


measured material

property?

Number of existing methods

Optical interference method and push-rod method

(TMA is included)

NMI/MRI activities

NIM (China), LNE (France), NMIJ

(Japan), KRISS (Korea), NPL

(UK),



for traceability?



Traceability issues

Supply of certified reference material is the

traceability rote for thermal diffusivity.

Calibration – reference materials

NMIJ (Japan), NIST (USA), PTB (Germany)

Uncertainty

Uncertainty budgets have been developed for these

measurements by NMIJ, Japan

Are there important


problem is not

addressed?

A few round robin measurements

were performed among research

institutes using the laser flash

method.

NMIs did not participated in these

measurements and the

measurements were not SI

traceable.

What is the way

forward?

CCT WG9 “Thermophysical property” covers

Thermophysical properties.

Round robin measurement of

thermal expansivity of gauge block

is under progress by CCL.

21


Table C4b Specific Heat Capacity

Specific heat

capacity

Issue / Evidence Comment / Plan

Heat capacity (Cp) All materials in liquid, micro, macro, particle, bulk

states

Is the material

property important?

Regulation Need

Cp of heat exchanger fluids necessary to determine

efficiency of thermal engines

Cp of building materials for fire protection

Uncertainty. Often 5 % is sufficient

Accreditation needs

Accredited testing laboratories for Cp testing need

traceability

For example, in Europe the

automobile industry has very

specific requirements on the

testing method. It is there

way to ensure comparability.

Aviation industry needs

traceable und comparable

results

Is there a problem

with consistency /


measured material

property?

Some discussion can be found in the literature

concerning apparent difference between drop

calorimetric results and adiabatic calorimetric

results (freezing in of defects)

Measurement with

calorimeters - DSC:

commercial, high uncertainty,

calibration with reference

materials. Adiabatic

calorimeters: low uncertainty,

traceable. Drop calorimeters:

low uncertainty, traceable,

high temperature range.

AC and pulse calorimeters:

suitable for low temperatures

Is the problem

caused by an


traceability?

Traceability issues - No traceability acc. to state of

the art. Good literature values exist for a number of

standards, e.g. Al2O3, Cu. no uncertainty budget.

Calibration – reference materials - yes

Uncertainty - yes, see D. Archer, 1993

What other aspects

are relevant to the

problem?

Standardized by standardization organizations like

ISO, DIN, ASTM etc.: 2 methods: DSC and drop

calorimetry ASTM E 1269: 2005: Standard Test

Method for Determining Specific Heat Capacity by

Differential Scanning Calorimetry: reproducibility:

8 %, repeatability: 6 %

ASTM E 968: 2002: Standard Practice for Heat

Flow Calibration of DSCs

DIN 51007: 1994-06: Thermal analysis;

differential thermal analysis; principles

DIN 53545: 1990-12: Determination of low-

temperature behaviour of elastomers; principles

and test methods

EN 821-3: 2005-04: Advanced technical ceramics

- Monolithic ceramics - Thermo-physical

properties - Part 3: Determination of specific heat

capacity

and many more material specific standards, mostly

without information about uncertainty

NMIJ/NMI activities

NIST: see D. Archer

PTB: setup of adiabatic

calorimeter

LNE: setup of drop

calorimeter

Are there important


problem is not

addressed?

What is the way

forward?

Thermophysical properties are covered by CCT

WG9 “Thermophysical property”

22


Table C5b Glass Transition Temperature

Transition Temperature Issue / Evidence Comment / Plan

Material Property Glass-transition temperature Is the material property important?

(e.g. does it have importance in

trade, regulations, etc.?).

This material property is used extensively in the

high performance composite arena to access the

shelf-life and completeness of cure of thermoset

based resin matrices. The measurement is often

made by dynamic mechanical analysis (DMA). Is there a problem with consistency

/ comparability of the measured

material property?

It has been shown in round-robin studies that

reproducibility of these measurements is poor,

with many degrees variation in reported values. Is the problem caused by an


Currently there is no traceability of the specimen

temperature to a commensurate degree as the

result is required. Need is for (say) 1C, but

errors can be 5-20 degrees. What other aspects are relevant to

the problem?

This property can also be obtained from

dielectric, DSC, thermal expansion

measurements. These methods do not provide

equivalent data. Are there important consequences

if this problem is not addressed?

(e.g. Can the financial or regulatory

impact of the issue be estimated?)

The materials subjected to this test are mainly

those at the high cost end of composites. The

consequences of measuring incorrectly, and

thereby over-estimating the degree of cure or

that a material is within shelf-life are very

serious as these materials are used increasingly

in high-performance applications (e.g.

commercial and military aircraft) What is the way forward?

(e.g. Is the property covered by an

existing CC? (Inform and offer to

support any work they initiate?), Is

it suitable for VAMAS, a standards

development organisation, or a

regional metrology organisation

(Euromet) activities?, Is work in

conjunction with CIPM and/or

ILAC necessary?, Is a reference

material needed? )

Although, the reported value is a temperature,

the actual temperature accuracy is not the

highest as an accuracy of 0.5 to 1 C provides a fit

for purpose value. There is a need to ensure that

test equipment and operators can provide correct

data. A pilot study should be undertaken in

conjunction with ILAC and CIPM.

23

ANNEX D TASK GROUP 3 – COMPOSITION and MICRO-STRUCTURAL

Table D1a To be added

Table D1b Grain Size

Grain size Issue / Evidence Comment / Plan

Material Property Grain size (average diameter, average area,

number of grains per unit volume or area,

average intercept length, standard grain size

number).


important? (e.g. does it have

importance in trade,

regulations, etc.?).

Yes, material properties and performance depend

on grain size, but no evidence of trade,

regulatory, or accreditation needs or drivers.


consistency / comparability

of the measured material

property?

No evidence of a problem with consistency /

comparability when the method used to

determine and express grain size is provided.



traceability?

No.



Quantitative microscopy techniques are the

primary methods for measuring grain size in

conventional materials. Methods for very fine

grain materials (submicron) include x-ray

(systematic peak broadening) and transmission

electron microscopy techniques.

Are there important


problem is not addressed?

(e.g. Can the financial or

regulatory impact of the

issue be estimated?)

No evidence that there are.


(e.g. Is the property covered

by an existing CC? (Inform

and offer to support any

work they initiate?), Is it

suitable for VAMAS, a

standards development

organization, or a regional

metrology organization

(Euromet) activities?, Is

work in conjunction with

CIPM and/or ILAC

necessary?, Is a reference

material needed? )

No evidence to suggest that customers have

significant metrological issues related to

measuring grain size. No obvious role for the

CIPM.

24


Table D2b Phase

Phase Issue / Evidence Comment / Plan

Material Property Phase (identification of one of the pure

compounds present in a material, including

chemical composition and arrangement)

Is the material property important?

(e.g. does it have importance in trade,


Important, but varies widely with industry

and application. No evidence of regulatory

or accreditation needs or drivers.

Is there a problem with consistency /

comparability of the measured

material property?

No evidence of a problem with consistency /

comparability. Users need low cost, ease of

use, user-friendly data interpretation

software, and databases of known quality to

identify unknown materials.



No.

What other aspects are relevant to the

problem?

Routine methods include x-ray diffraction

for crystalline materials augmented by

electron microscopy methods. Non-routine

methods include neutron diffraction and

synchrotron-based methods.

Are there important consequences if

this problem is not addressed? (e.g.

Can the financial or regulatory

impact of the issue be estimated?)

No evidence that there are.


(e.g. Is the property covered by an

existing CC? (Inform and offer to

support any work they initiate?), Is it

suitable for VAMAS, a standards

development organization, or a

regional metrology organization


conjunction with CIPM and/or ILAC

necessary?, Is a reference material

needed? )

No evidence to suggest that customers have

significant metrological issues related to

measuring phase. No obvious role for the

CIPM.

25


Table D3b Porosity

Porosity Issue / Evidence Comment / Plan Material Property Porosity (pore size, pore size

distribution, specific surface area)

Is the material property important? (e.g.

does it have importance in trade,


Yes, for catalysts and sintered

materials and for the effectiveness of

pharmaceutical and chromatographic

carriers; important in quality control;

important in the electronics, paper,

and concrete industries. No evidence

of regulatory or accreditation needs

or drivers.

Is there a problem with consistency /

comparability of the measured material

property?

Yes, to the extent that standards

development organizations such as

ASTM International, BSI, DIN, and

ISO develop and maintain numerous

standards in this area, and

organizations such as BAM, BCR,

LGC, and NIST develop and provide

reference materials.

Is the problem caused by an unaddressed

need for traceability?

No evidence to suggest that it is. What other aspects are relevant to the

problem?

Numerous methods exist for

measuring porosity in different

materials under different

circumstances, e.g., gas adsorption,

mercury intrusion, fluid flow, neutron

scattering, x-ray scattering, electron

microscopy, NMR, others.

Are there important consequences if this

problem is not addressed? (e.g. Can the

financial or regulatory impact of the issue

be estimated?)

No evidence to suggest new

consequences if the problem is not

addressed by the CIPM.

What is the way forward? (e.g. Is the

property covered by an existing CC?)

(Inform and offer to support any work

they initiate?), Is it suitable for VAMAS,

a standards development organization, or

a regional metrology organization


conjunction with CIPM and/or ILAC

necessary?, Is a reference material

needed? )

Suitable for standards development

organizations and VAMAS and

developers of reference materials. No

obvious or compelling role for the

CIPM, at least at this time.

26


Table D4b Crystalline Texture

Crystalline Texture Issue / Evidence Comment / Plan

Material Property Crystalline texture (uniaxial, typically developed

in thin films and rods; three dimensional,

typically developed in rolled sheets of metal)





Important in the hard disk drive industry and in

nanofabrication and nanomechanics. No

evidence of regulatory or accreditation needs or

drivers at this time.



the measured material

property?

Little known activity in the development of

either documentary standards or reference

materials for texture per se. No evidence of a

problem with consistency / comparability.



traceability?

No evidence to suggest that it is.


to the problem?

Are there important


is not addressed? (e.g. Can

the financial or regulatory

impact of the issue be

estimated?)

No known consequences if not addressed by the

CIPM.


(e.g. Is the property covered by

an existing CC? (Inform and

offer to support any work they

initiate?), Is it suitable for

VAMAS, a standards


regional metrology

organization (Euromet)

activities?, Is work in


ILAC necessary?, Is a

reference material needed? )

May be suitable for standards development

organizations and VAMAS and developers of

reference materials. No obvious or compelling

role for the CIPM, at least at this time.

27


Table D5b Particle Size

Particle Size Issue / Evidence Comment / Plan

Material Property Particle properties Size and concentration are considered

most important from the viewpoint of

metrology. In some specific areas,

other properties such as surface area

and density are important as well.


important? (e.g. does it

have importance in trade,


1. Traceable measurement of particle

concentration (in terms of number or

mass) is being required for regulating

Diesel nanoparticle emissions.

2. Traceable measurement of particle

size and concentration is being

required from the safety concern

about engineered nanoparticles

(concern about so called "nanorisk").

3. Particle size and concentration

have been important issues in powder

and pharmaceutical industries (for

quality control), and semiconductor

manufacturing (for contamination

control).

Discussions on regulating Diesel

nanoparticles have been made by the

United Nations GRPE (Working

Party on Pollution and Energy) for

several years.




Inconsistency is frequently observed

among measurement results for

particle size distributions and

concentrations.

This problem has rarely been

addressed from the traceability

viewpoint.



traceability?

Yes. Traceability in particle size is

established and maintained in only

few countries. There is no traceability

established for particle number

concentrations.

Research to establish a measurement

standard of particle number

concentration is being conducted in

some NMIs.


to the problem?

Are there important


not addressed? (e.g. Can the

financial or regulatory impact of

the issue be estimated?)

Regulation on Diesel nanoparticles

attempted in the UN GRPE may lose

technical grounds, if no traceability is

established for particle concentration.






VAMAS, a standards


regional metrology organization




material needed? )

No CCs, nor other organizations,

have covered the traceability of

particle properties so far. It will be

desirable for experts of particle

measurements in NMIs to meet and

discuss the issue.

Because size is not the only issue in

particle properties, CCL will not be

an adequate place to discuss the issue

in. We need to organize

interlaboratory comparison for nano-

particle size covered by an

appropriate CC to evaluate

comparability between NMIs or other

major organizations. VAMAS can

give many private companies a

suitable opportunity to contribute

standardization and international

comparability.

28


Table D6b Defects

Defects Issue / Evidence Comment / Plan

Material Property Defects (crystalline lattice defects, including

extended and point defects; and microscopic

defects, including inclusions and cracks)





There are numerous measurement needs related

to defects, expressed by multiple industries.

Defects are called out as a key challenge for

nanoelectronics, photonics, and magnetics. User

needs include assessment of defect type, number

density, and statistical characteristics of defect

populations. Two common themes: sensors, in-

line monitoring. No evidence of regulatory or

accreditation needs or drivers at this time.




property?

Little known activity in the development of

either documentary standards or reference

materials for defects per se, especially for

crystalline defects. Numerous comparisons of

different techniques, but usually semi-

quantitative.



traceability?

No.



Numerous and diverse methods exist for

measuring both crystalline and microscopic

defects.

Are there important





estimated?)

No known consequences if not addressed by the

CIPM.


(e.g. Is the property covered

by an existing CC? (Inform

and offer to support any work

they initiate?), Is it suitable for

VAMAS, a standards


regional metrology

organization (Euromet)





May be suitable for standards development

organizations and VAMAS and developers of

reference materials. No obvious or compelling

role for the CIPM, at least at this time.

29

ANNEX E TASK GROUP 4 – FUNCTIONAL PROPERTIES

Table E1a To be added

Table E1b Dielectric Properties: permittivity

Complex

permittivity

Issue/Evidence Comment /

Plan Scope Complex permittivity

Material

Category

Ceramic, polymer, composite, rubber, organic

State and Scale Bilk, liquid, film, micro, nano, (surface)

Regulation Need 1) Dielectric reference liquids used in mobile communications for SAR

(specific absorption rate). 2) Insulation oils for transformers (conductivity

limits). 3) MRI scans – Hugo model – phantom solid tissue equiv.

Phantoms currently employs dielectric liquids. 4) Dielectric approach to

moisture measurement is common, but lacks standardisation.

User needs Insufficient accuracy of dielectric input data in electromagnetic

modelling (e.g. modelling of radomes, antennae, bio-tissues).

Accreditation

needs

UKAS laboratories – small number in past

Yes, see SAR above – reference liquids. Comparability

Some NPL published data on liquids – NIST now starting work (note:

sources of reproducible solid reference material are difficult e.g. pure

quartz, YAG, otherwise batches of material must be traceably measured)

Euromet 685 on solids – laminar dielectrics. Need for

intercomparison (possibly a WGMM could follow 685 depending on results).

Economic impact

studies

No known data, but case could be made in comms. and defence area as

the technology depends on dielectric materials. SAR is a major potential

risk risk.

Number of

existing methods

Many, but most are too loose in detail to be useful for full traceability and

to guarantee reproducibility between labs. There are some good standards

for specific technical measurements (where industrial reproducibility is

more important than absolute accuracy). SAR standards are relatively

new & good as they had real metrological input.

Standardisation

situation

Many obsolete standards (except key areas such as SAR: IEEE Standard

1528-2003, ISBN 0-7381-3716-2, CENELEC standard EN 50361:2001,

IEC Standard 62209-1, 2005)

NMI/MRI

activities

Euromet 685 involves NIST, VNIIMS, NPL, BAM and Polish designated

lab (Technical University of Warsaw).

R & D phase? Rf & Microwave: general movement into smaller scale (e.g. micro)

measurements. Low frequency (LF) research on nano-composites,

breakdown, electrokinesis, etc.

Traceability

issues

NMIs ensure traceability, but most industry and academic. RF &

microwave measurements are not traceable.

SI units relevant Microwave: length (dimensions, displacement), time (frequency), LF &

RF via impedance/capacitance.

CCs coverage CCEM

Prior studies Intercomparisons every so often – informal results available.

Method

comparability

See above

Standard test

machines

Mostly bespoke (i.e. different cell sizes)

Calibration –

reference

materials

Reference liquids (controlled by composition). Very few solid material

standards, though most measurements on solids – only pure crystals

suitable.

Uncertainty NMIs promote this- 2003 meeting on Dielectric Measurement

Uncertainties.

30


Table E2b Electrical Properties

Electrical properties Issue / Evidence Comment / Plan Material Property Dielectric These comments apply to the

RF, Microwave and THz regions

of spectrum





Traceable measurement of dielectric

properties is stipulated in international

standards Health and Safety standards

relating to RF interactions with humans

(e.g. RF generated by mobile phones) and

in 2008 the EC Physical Agents (EMF)

Directive will require all employers to

abide by these standards. There is a more

general problem of supplying good

quality dielectric data as input to EM

field-modelling programmes: these days

the algorithms are of good quality and the

predicted performance of

component/system designs is often

limited rather by the large uncertainties

and/or errors in the dielectric data.

Computer-based EM field

modelling is widely used by

European electronics-based

industries.




property?

Yes, measurement comparisons between

labs often exhibit discrepancies, which

exceed joint estimated uncertainties -

sometimes to a considerable extent.

Education of those involved in

dielectric measurements should

help: the dielectrics community

is in general far less aware of the

value of realistic uncertainty

estimation than other

metrological disciplines are.



traceability?

In some cases, yes. Many existing

dielectric measurement standards do not

mention the need for traceability



The large number of degrees of freedom

that dielectric measurements suffer from

measurements (e.g. types of material,

frequency range, temperature, moisture,

available specimen size) makes it difficult

and potentially costly to standardise good

practice over a very wide field.

Are there important





estimated?)

Performance of systems will not be

optimised. In some cases Health & Safety

may be compromised






VAMAS, a standards


regional metrology

organisation (Euromet)





A microwave measurement comparison is

currently being run by the Euromet High

Frequency Electromagnetics Sub-field,

which may highlight some of these

problems (Internationally it comes under

the remit of CCEM).

Growing demand from industry

for better measurements may

trigger a need for a more

comprehensive programme of

international metrology here.

31

Table E3a Magnetic Properties

Magnetic Properties Scope AC and DC B versus H properties and related quantities such as specific total loss and

relative magnetic permeability. Measurements made on a range of test specimen dimension

that meet material property requirements.

Material

Category

Bulk, laminates, soft magnetic composites, polymer-bonded permanent magnets.

Material State

and Scale

Bulk, 2D (laminates) nano-composite (permanent magnets)

Regulation

Need

IEC standards require the material properties to meet certain values and that standard

measurement methods are used to determine these.

User needs Users need material properties that are suitable for their application. Often this means making

measurements for conditions that are far from the laboratory. Standard methods underpin any

approach adopted.

Accreditation

needs

Manufactures of transformers have to meet certain energy loss requirements and the

underpinning measurement of specific total loss is traceable to National Standards.

Comparability A number of different measurement systems are used for the same magnetic quantity and

reproducibility is extremely important.

Need for

intercomparison

If a suitable quantity could be identified and a suitable reference standard established then the

community would benefit from such an activity.

Economic

impact studies

Not aware of any, although electrical steel manufacturers presumably have such information.

Number of

existing

methods

The IEC have a number of standards covering magnetic measurements and the number is

growing as new measurement techniques reach FDIS status. NPL can provide measurements

compliant with 7 standards.

Standardisation

situation

See last statement – Lowest measurement uncertainties possible are required.

NMI/MRI

activities

PTB have a similar capability.

R & D phase? UK project finishing March 08 developing a measurement method for the AC properties of

soft magnetic materials for operational waveforms, under stress and at elevated temperatures

applied simultaneously.

Traceability

issues

Each of the discrete instruments used in the measurement system has a suitable calibration.

Examples are calibrated micrometers, calibrated mass balance, calibrated resistors and

calibrated digital voltmeters.

SI units relevant All are derived units.

CCs coverage Properties have a number of CC entries.

Prior studies A CCEM comparison of magnetic field strength (the required H) was performed using a

special solenoid as the transfer standard.

Method

comparability

Bilateral measurements with PTB have been performed for specific total loss.

Standard test

machines

No - measurement systems are established from discrete instruments.

Calibration –

reference

materials

Reference cores calibrated to the users requirements.

Uncertainty Uncertainty budgets exist for all material measurements that have CC entries.

32

Table E3b Magnetic Properties

Magnetic Properties Issue / Evidence Comment / Plan Material Property e.g. Magnetic Property - Specific Total Loss



importance in trade, regulations,

etc.?).

Determines the energy loss in electrical

machines and other devices. Accurate

measurement of this quantity is required for

future energy efficient applications.

Units -




Measurement of specific total loss requires a

magnetic circuit and the realisation of this

circuit is a known problem. New materials are

measured using a different circuit and this

makes comparisons difficult.






VAMAS, a standards






material needed? )

An CC exist for Epstein and Single Sheet

measurements at 50 and 400 Hz.


to the problem?

Conditions of material use are key.

Measurements are made for standard

conditions but the material is used in an

environment that is very different.

Effect of stress

Are there important


not addressed? (e.g. Can the

financial or regulatory impact of


Without traceable measurements to develop

the materials and optimise device performance

considerable energy will be wasted. With the

move to more electric transport being driven

by environmental issues the impact is large

and far-reaching.






VAMAS, a standards






material needed? )

An WG exist for Epstein and Single Sheet

measurements at 50 and 400 Hz.

33

Table E4a Optical Properties

Optical - Fluorescence

Scope Fluorescence lifetime, intensity (quantum yield) & spectrum

Material Category Biological, Organic LED materials

Material State and

Scale

Liquid (dyes), micro (cells), particle (single particle), bulk (e.g. dyes on textiles, dried

paints), film (OLED), nano (cell structures)

Regulation Need Not aware of any at present

User needs What are the user requirements? Intercomparisons in biological studies, product

development (pharmaceuticals, OLEDs), new molecular probes, or old probes in “new”

environments

Accreditation needs Not sure

Is there a need for comparability of data? Comparability

Yes (e.g. in clinical diagnostics)

Need for

intercomparison

Fluorescence lifetime imaging (instrument manufacturers, research labs), Quantum yield

(NMI’s)

Economic impact

studies

Not sure

5 methods for Quantum yield (most common: comparison with ref standard);

2 methods for lifetime (time or frequency based);

Number of existing

methods

spectrum (scanning or array system)

Quantum yield ref standard (quinine sulphate calibrated by NIST) Standardisation

situation Spectral ref standards (fluorescein calibrated by NIST, proprietary standards sold by BAM,

commercial proprietary standards)

NMI/MRI activities Recent NIST/NRC/BAM spectral intercomparison (2005)

R & D phase? Single-molecule spectroscopy

Spectra via reference standard materials; Traceability issues

None for lifetime standards

SI units relevant None

CCs coverage No

Prior studies

(method specific)

(ref standards described above, NMI intercomparison…)

Method

comparability

Standard test

machines

Yes, commercial instruments available for lifetime, spectrum and quantum yield

Calibration –

reference materials

Yes, see above

Uncertainty Yes, for reference materials

34

Table E4b Optical Properties

Optical Properties Issue / Evidence Issue / Evidence Issue / Evidence

Material Property Apparent texture (i.e.

texture as manifested

optically)

Gloss

Colour


important? (e.g. does it

have importance in

trade, regulations,

etc.?).

Yes, apparent texture

affects consumer trade

Yes, e.g. where it

affects or determines

visibility of displays

Yes, colour matching

and perception

important for consumer

trade


consistency /


measured material

property?

There is currently no

standard measurement

to enable apparent

texture comparisons

Commercial gloss

meters exist, but are

based on a very small

subset of possible

measurements.

Therefore comparing

materials through gloss

meter measurements is

often misleading or

uninformative.

Not in terms of the

standard colour

measurements, which

commercial instruments

can make. However,

“apparent” colour (i.e.

both colour rendering in

different lighting

situations and

appearance of coloured

objects in different

surrounds) can lead to

problems. Colour

rendering issues are the

leading cause of

products being returned

to shops.



for traceability?

No scale or traceability

exists at present

Traceability exists, but

addresses only specific

gloss meter measure-

ment(s) rather than a

full characterisation of

glossiness

The problems raised

above are well known,

but to date no

traceability chain exists.



Apparent texture is

correlated with physical

texture.

Some increasingly

popular materials

coatings (e.g.

interference pigments)

have a viewing-angle-

dependent colour.

Are there important


problem is not

addressed?

(e.g. Can the financial

or regulatory impact of


There would be

positive consequences

to developing standards

(e.g. to specific

industries such as CGI

or decorative surface

manufacturers), but it’s

hard to estimate

negative consequences

if these are not

developed in the near

future.

Probably not major, so

long as custom

measurements can be

made when required.

There is a financial

impact to industry, but

it’s hard to estimate

What is the way

forward? (e.g.

undertake a round-

robin, develop a

reference procedure,

develop and validate a

reference material,

research a new method)

Develop reference

procedures and/or a new

method.

Develop reference


method

Develop reference


method. .

35


Table E5b Acoustic Properties

Acoustic

Properties

Issue / Evidence Comment /

Plan Scope Speed of sound, attenuation and/or absorption, or scattering cross-

section measurements of materials, typically tissue-mimicking

(TMM) or tissue-like materials.

Material Category Water based gelatin, loaded with scattering materials to generate

the ‘correct’ properties.

Material State and Scale Macro, semi-solid – samples will be typically 50 mm � and 10

mm – 40 mm thick.

Regulation Need The properties of the TMM material are specified in and IEC

Standard for realising a reference flow phantom for testing

Doppler ultrasound equipment and for use in a thermal test object

(used to measure temperature rise generated by medical ultrasound

equipment).

User needs Uncertainty: fit-for-purpose. Most user requirement relate to

uniformity and ease-of-manufacture and medium and long-term

stability.

Accreditation needs No.

Comparability Not sure.

Need for

intercomparison

I would anticipate that, if it is felt that such a comparison between

NMIs is important, then this will be done through the CCAUV.

Economic impact

studies

No.

Number of existing

methods

Currently, none.

Standardisation

situation

None.

NMI/MRI activities Probably carried out in underpinning other projects.

R & D phase? Yes for scattering cross-section: For other properties: no, not

really.

Traceability issues This is a relative measurement, carried out with reference to a

standard liquid, water, whose properties are well established.

SI units relevant Sample thickness is an important measurement.

CCs coverage Probably CCAUV.


specific)

Purely informally, as part of an EU project, but also through a UK

intercomparison which used reference oils. Also, a comparison of

TMM properties was carried out in the US.

Method comparability No.

Standard test machines None. Have machines been compared? No.


materials

NPL has provided these in the past, on a limited scale (these are

based on reference oils – Dow Corning-710 oil).

Uncertainty Yes, within NPL, for attenuation and speed-of-sound.

36

ANNEX F TASK GROUP 5 – ELECTROCHEMICAL PROPERTIES

Table F1a To be added

Table F1b Electrochemical Properties

Electrochemical Issue / Evidence Comment / Plan

Material Property Corrosion 1 (Electrochemistry)


important? (e.g. trade,

regulations)

Corrosion is a major reason for materials failure

and economic loss;


consistency /


measured material

property?

The measurement of corrosion rates is mainly

based on mass loss, optical analysis and

electrochemical measurements of corrosion

currents. Measurements mainly rely on standards

with well-established boundary conditions and

well-characterised materials. Data are available

for certain standards and established materials in

certain corrosive environments. Problems arise

for new materials, the prediction of corrosion

behaviour on the basis of accelerated tests and

for new corrosive environments.

In polycrystalline materials the different

grain orientations and thereby induced

different local surface energies and

reactivities are often leading to locally

varying corrosion phenomena. This will

strongly influence the corrosion of the

material as whole. Resolving this

question will lead to more reliable

corrosion measurement and improved

corrosion protection.



for traceability?

No. Development of methods to detect the

evolution of very thin (nanoscale)

protective layers of economic relevance

for new materials is required.



Materials are complex in the variability of their

microstructure, orientation and composition of

grains, leading to local reactivity. Particularly, as

corrosion is concerned, these materials

properties cannot be generalised but extremely

specific for the interplay between materials

structure and environmental conditions.

Bridging the gap between high

precision electrochemical, microscopic,

optical and spectroscopic measurements

and routine testing procedures applied

in industry.

Are there important


problem is not

addressed? (e.g. Can

the financial or

regulatory impact of the

issue be estimated?)

If the problem of advanced corrosion analysis is

not addressed, lifetime prediction of new

functional materials and the prediction of the

influence of the release of materials on their

environment (e.g. human body in case of

implants, …) will not be possible. This

significantly hampers the development of new

materials and therefore has a dramatic economic

and ecological impact.

What is the way

forward? (e.g.

Is the property covered

by an existing CC?

(Inform and offer to

support any work they

initiate?), Is it suitable

for VAMAS, a

standards development

organisation, or a

regional metrology

organisation (Euromet)


conjunction with CIPM

and/or ILAC

necessary?, Is a

reference material

needed? )

The existing knowledge and standards do not

sufficiently allow to understand the grain

orientation dependant corrosion rates (e.g.

surface energy and etching rate and surface

chemistry are often grain orientation dependant).

However, most engineering materials are

polycrystalline and the texture is designed with

regard to functional properties). CCs addressed

are CC-Length, CC-Electricity and Magnetism,

CC-Mass and Related Quantities and CC-

Amount of Substance - Metrology in Chemistry.

The scientific implications should be treated in a

VAMAS working group. The relevance for

trade, standardization and international rules for

quality and trade might be treated by ILAC

To solve this issue it is suggested to

combine the methods EBSD (electron

backscattering diffraction) with

profilometry on the nanoscale (best

suited method to be determined) and

local optical metrology for thickness

analysis of formed oxide films. In an

initial phase the orientation of grains in

polycrystalline material and individual

dissolution (corrosion) rates should be

measured and correlated. In a second

stage, by means of spectroscopy, the

evolution of protective thin layers have

to be assessed and applied to the

observation of corrosion depending on

the crystal orientation. Finally, the

combination of the topographic and

optical methods should lead to a better

prediction and control of the

polycrystalline corrosion behaviour.

37

ANNEX G PILOT STUDIES (outline proposals)

G1. MEASUREMENT OF MODULUS ROUND ROBIN

Introduction

In spite of the long history of testing metals, recent experience suggests that the measurement of

modulus is not trivial and there can be large discrepancies in the values measured even from

experienced practitioners. Currently the only standard available for measuring the Young’s

modulus of metals from the tensile test is ASTM E111, and there are many issues that contribute to

the variability, which still need to be addressed. The European TENSTAND project reported on

the accuracy of modulus measurement from the conventional tensile test, with recommendations

for a separate procedure for modulus measurement, but this has not been progressed. Work has

been carried out in the past on metal matrix composites, which has also highlighted strain

measurement and data analysis as key factors affecting the quality and accuracy of the results.

Dynamic methods are sometimes used, but the tests are primarily those developed for the testing of

ceramics.

There are also issues with the testing of modulus at temperature, where reliable data and test

methods are not available.

Although there are no reference materials specifically developed for modulus measurement, a BCR

Nimonic 75 tensile reference material does exist. This has not been fully certified for modulus; and

the proposal within this exercise is to examine the tensile and dynamic modulus techniques with

the aim of validating and certifying the material for modulus measurement.

Round-robin organisation

•Source BCR Nimonic tensile reference material and prepare test pieces.

•Circulate manufactured test pieces for tensile and dynamic measurement

•Specify test conditions – alignment, loading, strain measurement and data analysis

•Collate results and report

•Report Young’s Modulus

Time schedule

•Sign up for the study:

•Distribution of samples:

•Reporting:

38

G2. GLASS TRANSITION (Tg) OF CURING RESIN SYSTEMS

Introduction

One example of materials metrology is the measurement of Tg - the glass transition temperature,

which is a materials property but reported as a temperature value, which is actually determined

through a wide range of other measurement techniques, including:-

- ultrasonics,

- dielectrics,

- calorimetry (DSC)

- expansion

- mechanical vibration (DMA)

- optical coherence tomography (OCT)

The value of Tg is often used as in materials qualification and specification requirements, as Tg is

related to service temperature capability. See Standard Qualification Plan.

These above techniques are all used as secondary measures of degree of cure and shelf-life. Some

of these techniques are better for off-line, rather than on-line measurements.

Standards exist for DSC (ISO 11357-3/ASTM E 1356), DMA (ISO 6721-11, ASTM D 3418). No

standards for Tg by ultrasonic, dielectric, calorimetry and OCT.

NPL has a project to calibrate these techniques for material of different cure state against a

"chemical" measure of cure (e.g. FTIR).

Round-robin activities

Supply panel of fully cured material

Glass-transition temperature to be determined by a range of techniques, as above.

Note NPL will supply a temperature reference specimen for calibration of DMA equipment.

Report

Report the glass-transition temperature

Time schedule

6-12 months

39

G3. MAGNETIC MEASUREMENTS ON NPL REFERENCE CORE T1002

An outline proposal for measuring magnetic properties is given below.

DC MEASUREMENTS

• Measure the normal magnetization curve and from this determine the maximum relative

magnetic permeability.

• Determine the B versus H hysteresis curve up to a magnetic field strength of 2200 A/m.

• From the measured B versus H hysteresis curve determine the remanence, Br, and the

magnetic flux density coercivity, HcB.

• The values determined should be sent to the organiser along with the estimated uncertainty

in these values within one month of completing the measurements.

AC MEASUREMENTS

• Measurements to be made at a frequency of 50 Hz. For all measurements the secondary

voltage waveform should be sinusoidal as defined in BS EN 60404 parts 2 and 3.

• Determine the specific total loss, Ps, and the specific apparent power, Ss, at peak values of

the magnetic flux density, Bpeak, of 1.0 T, 1.1 T, 1.3 T, 1.5 T and 1.6 T.

• Determine the peak magnetic flux density, Bpeak, for a peak magnetic field strength of 1000

A/m.

• The values determined should be sent to NPL along with the estimated uncertainty in these

values within one month of completing the measurements.

The following physical data can be assumed for the measurements:

Mass of core = 0.5075 kg

Cross-sectional area of core = 1.5030 × 10 -4

m2

Mean magnetic path length of core = 0.44061 m

Number of primary turns = 300

Number of secondary turns = 150

N.B. While the windings are identical, the left pair of secondary terminals (when viewing the core

with the secondary terminals at the top) should be used.

To limit contributions due to temperature coefficients, the properties of the core should be

measured for an ambient temperature of 20 ± 1 °C.

The laboratory should follow their own technical procedure for measuring the required properties.

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