Diapositive 1 - LBMA 2019/6. Reference Materials - Jo… · ISO 17034 Structure General requirements 7.2 Production planning 7.3 Production control 7.4 Material handling and storage

ISO 17034

Accreditation for

Reference Materials Makers

Jonathan J. Jodry

Head of Laboratories & New Business Development

Metalor Technologies SA, Switzerland

LBMA Assaying and Refining Conference

March 2019, London

Conclusion

The quality of your analysis

can never be better

than the quality of

your proofs & standards

Au 999.8 with specific impurity levels

Monoelemental solution of Ag 1 mg/L

Pd 500 alloy

Pt-Ir alloy for hardness

Au 750 alloy 3N for colour reference

Pure substances characterised for chemical

purity and/or trace impurities.

Standard solutions and gas mixtures

Matrix reference materials, characterised for

the composition of specified major, minor or

trace chemical constituents.

Physico-chemical reference materials

characterised for properties such as melting

point, viscosity, and optical density.

Reference objects or artefacts characterised

for functional properties such as taste,

odour, octane number, flash point and

hardness.

Reference Materials – Definition

A Reference Material is

a sufficiently homogeneous and stable material

relative to one or more properties

and is prepared for analytical purpose

Examples:

Usage of Reference Materials

calibration, re-

calibration & proof

requirement of

ISO 17025

standard

assessing

performance

of the

laboratory

validating new

analytical

methods

round

robins

detection

of errors


Cupellation Potentiometry

proof proof


Cupellation Potentiometry ICP-OES SPARK-OES XRF

calibration calibration calibration

re-calibration re-calibration

proof proof

ISO Deliverables

ISO/PAS – Publicly Available Specification

ISO/TS – Technical Specification

ISO/TR – Technical Report

ISO International Standard

ISO Guides

ISO Deliverables

ISO Guide 30 Reference materials -- Selected terms and definitions

ISO Guide 31 Reference materials -- Contents of certificates, labels and

accompanying documentation

ISO Guide 32 Calibration in analytical chemistry and use of certified reference

materials

ISO Guide 33 Reference materials -- Good practice in using reference materials

ISO Guide 34 General requirements for the competence of reference material

producers

ISO Guide 35 Reference materials -- Guidance for characterization and assessment of

homogeneity and stability

ISO/IEC Guide 2 Standardization and related activities -- General vocabulary

ISO/IEC Guide 50 Safety aspects -- Guidelines for child safety in standards and other

specifications

ISO Guide 82 Guidelines for addressing sustainability in standards

ISO Guides

ISO 17034 Environment

ISO Guide 31Documentat.

for RMs

ISO Guide 35Characteris. & Certification of

RMs

ISO Guide 30Definition & Terminology

related to RMs

ISO Guide 33Uses of RMs

ISO Guide 34Competence

of RMs producers

TR 79RMs for qualitative analysis

TR 10989Guidance on RMs

TR 11773Distribution of RMs

TR 16476Establishing traceability of RMs

Until 2016… ISO structure related to Reference Materials



for RMs


RMs


related to RMs


ISO 17034Competence

of RMs producers





From 2016…



for RMs


RMs


related to RMs


ISO 17034Competence

of RMs producers





From 2016…

ISO 17034 Structure

ISO 17034

General requirements for the competence of reference material producers

ISO 17034 Structure

ISO 17034


4 General requirements

Contractual matters, Impartiality, Confidentiality

5 Structural requirements

6 Resource requirements

Personnel, Subcontracting, Services and supplies, Facilities

7 Technical and production requirements

8 Management system requirements

ISO 17034 Structure

ISO 17034


4 General requirements

Contractual matters, Impartiality, Confidentiality

5 Structural requirements

6 Resource requirements

Personnel, Subcontracting, Services and supplies, Facilities

7 Technical and production requirements

8 Management system requirements

ISO 9001 & ISO 17025 as prerequisite are strongly recommended!

This allows to cover most of chapters 4, 5, 6 & 8 requirements.

ISO 17034 Structure

General requirements

7.2 Production planning

7.3 Production control

7.4 Material handling and storage

7.5 Material processing

7.6 Measurement procedures

7.7 Measuring equipment

7.8 Data integrity and evaluation

7.9 Metrological traceability of certified values

7.10 Assessment of homogeneity

7.11 Assessment and monitoring of stability

7.12 Characterisation

7.13 Assignment of property values

7.13 Assignment of the uncertainties of the property values

7.14 RM documents and labels

7.15 Distribution service

7.16 Control of quality and technical records

7.17 Management of non-conforming work

7.18 Handling of complaints

ISO 17034 Structure

General requirements RMs CRMs

7.2 Production planning

7.3 Production control

7.4 Material handling and storage

7.5 Material processing

7.6 Measurement procedures

7.7 Measuring equipment

7.8 Data integrity and evaluation

7.9 Metrological traceability of certified values

7.10 Assessment of homogeneity

7.11 Assessment and monitoring of stability

7.12 Characterisation

7.13 Assignment of property values

7.13 Assignment of the uncertainties of the property values

7.14 RM documents and labels

7.15 Distribution service

7.16 Control of quality and technical records

7.17 Management of non-conforming work

7.18 Handling of complaints

Homogeneity

For each Reference Material produced, 2 questions have to be answered:

• Is the material homogeneous ?

• Is the homogeneity obtained fit for purpose?

Homogeneity assessment will depend on the usage of the material!

Homogeneous Heterogeneous

Typical example : an XRF Reference Material can be homogeneous with a measuring window of 2 mm,

but heterogeneous with a 0.2 mm window.

Homogeneity

For each Reference Material produced, 2 questions have to be answered:

• Is the material homogeneous ?

• Is the homogeneity obtained fit for purpose?

Homogeneity:

• Checked by ANOVA (ANalysis Of VAriance)

• Protocol cannot be changed & Outliers can usually not be removed

• Selection of part of the material is not acceptable

For a wire – 1 dimension

Homogeneity

Homogeneity:




This materiel is homogeneous – but displays a certain dispersion !

Homogeneity

df MS F F crit.

SSA - X 2892.407018 18 160.7 1.84 1.93

Homogeneity:




This materiel is heterogeneous – but completely fit for purpose !

df MS F F crit.

SSA - X 413.7522807 18 23.0 1.99 1.93

Homogeneity

Homogeneity:

• Situation is more complex when handling 3 dimensions!

This materiel is highly homogeneous, along all axes

Homogeneity

df MS F F crit.

SSA - X 1.757 5 0.4 2.07 2.37

SSB - Y 0.744 2 0.4 2.19 3.15

SSC - Z 0.095 1 0.1 0.56 4.00

SSAB - XY 5.383 10 0.5 1.95 1.99

SSAC - XZ 11.629 5 2.3 2.15 2.37

SSBC - YZ 0.952 2 0.5 2.81 3.15

SSABC - XYZ 5.414 10 0.5 1.42 1.99

SSE 12.213 72 0.2

SST 38.187 107

check 38.187 107

Property Values & Uncertainty

A Property Value is any property assigned to the

Reference Material. It has to be determined following an

ISO 17025 accredited method, or a strictly validated

method.

The Uncertainty evaluates the confidence level of each

property value

Refining

Metalor Technologies SA

Route des Perveuils 8, CH-2074 Marin-Epagnier, Sw itzerland

Tel: +41 (0)32 720 6111

Element Unit Value Uncert. Element Unit Value Uncert. Element Unit Value Uncert.

Au mg/kg 251.7 5.0 In mg/kg 27.5 1.5 Si mg/kg 27.9 2.7

Al mg/kg 15.2 0.9 Mg mg/kg 16.9 0.6 Sn mg/kg 27.7 0.9

As mg/kg 23.3 0.9 Mn mg/kg 35.1 1.2 Te mg/kg 23.6 1.3

Bi mg/kg 24.6 1.0 Ni mg/kg 34.1 1.6 Zn mg/kg 26.7 0.7

Ca mg/kg 7.2 0.7 Pb mg/kg 25.2 0.7

Cd mg/kg 24.7 0.8 Pd mg/kg 32.1 1.5

Co mg/kg 10.0 0.9 Pt mg/kg 15.3 0.7

Cr mg/kg 1.7 0.2 Rh mg/kg 17.2 2.4

Cu mg/kg 241.9 9.8 Sb mg/kg 25.8 1.2

Fe mg/kg 14.2 0.6 Se mg/kg 23.2 1.8 Total mg/kg 976.04 21.1

Metalor ID: MER18202

When available, certif ied values have been established w ith expanded uncertainty (UCRM = kuc, w here uc is the combined standard uncertainty

calculated w ith a coverage factor k=2 according to the ISO Guide to Expression of Uncertainty in Measurement , ISBN 92-67-10188-9, 1st ed.

ISO, Geneva, Sw itzerland (1993)).

Disclaimer

Metalor Technologies SA has used its best endeavours to ensure that this material is homogeneous in respect of the contained elements and

that all concentrations are accurately determined. How ever, all assayers w ill recognize that there can be no absolute guarantees in relation to

these parameters. For example, presence of extraneous inclusions or minor deviations from complete homogeneity w hich are not detected by

the homogeneity testing are conceivable. Technical support on this material can be obtained by contacting [email protected].

Storage and handling

Intended use

Uncertainty

Ag

Comment

Certificate of Analysis

Reference Material

The material and its certif ied property values are expected to remain unchanged for more than 50 years, but new analytical techniques or

instruments w ith better characteristics of accuracy and precision might appear, hence a 20-years period has been arbitrary f ixed.

Keep the material in a plastic box or bag, aw ay from dusts, metallic dusts or vapour w hich may deposit on the surface. The material can be

cleaned w ith ethanol follow ed by high-purity w ater. Surface contamination can be removed by follow ing the standard procedures defined for

the preparation of samples.

This material is intended to be used as SUS (setting-up sample) for SPARK-OES spectroscopy, and has an homogeneity appropriate for such

usage.

nnnnnnnnnn, Silver RMAg Disc, 2 Round discs min 20mm dia, thickness ±12mm

ICP-OES (accredited Method)


Production Date

Metalor Technologies SA has a Quality System certified by SQS

ISO 9001, ISO 14001, OHSAS 18001

Approved by

Dr. Jonathan J. Jodry

Head of LaboratoriesJune 2038June 2018

Uncertainty

0.02

Value

This report can only be reproduced in full and with the written approval o f the

laboratory. Any details concerning the analytical methods and the measurement

uncertainties can be supplied by the laboratory upon request. - FOR 1136, V. 1.00

All certificates available on www.metalor.com

Property Value & TraceabilityThis product is Traceable to NIST via an unbroken chain of comparisons. The uncertainties for each certif ied value are reported. All scales are

checked daily using an in-house procedure, and calibrated yearly. Traceability information can be obtained upon request.

page 1 of 1

Unit

‰

Expiration Date

999.024

Element

Element Unit Value Uncert. Element Unit Value Uncert. Element Unit Value Uncert.

Au mg/kg 251.7 5.0 In mg/kg 27.5 1.5 Si mg/kg 27.9 2.7

Al mg/kg 15.2 0.9 Mg mg/kg 16.9 0.6 Sn mg/kg 27.7 0.9

As mg/kg 23.3 0.9 Mn mg/kg 35.1 1.2 Te mg/kg 23.6 1.3

Bi mg/kg 24.6 1.0 Ni mg/kg 34.1 1.6 Zn mg/kg 26.7 0.7

Ca mg/kg 7.2 0.7 Pb mg/kg 25.2 0.7

Cd mg/kg 24.7 0.8 Pd mg/kg 32.1 1.5

Co mg/kg 10.0 0.9 Pt mg/kg 15.3 0.7

Cr mg/kg 1.7 0.2 Rh mg/kg 17.2 2.4

Cu mg/kg 241.9 9.8 Sb mg/kg 25.8 1.2

Fe mg/kg 14.2 0.6 Se mg/kg 23.2 1.8 Total mg/kg 976.04 21.1

Ag



Uncertainty

0.02

ValueUnit

‰ 999.024

Element

Traceability

Full traceability is required for Certified Reference Materials only

Example for Trace Analysis by ICP-OES:

Matrix element

Mono-elementalsolutions addition

Validation by

bracketing

Traceable

to NIST

ISO 17034

RM

Analysis of CRM

with validated

and traceable

standards

All steps, all instruments and all materials

have to be registered

F u l l t r a c e a b i l i t y

Why use ISO 17034 Reference Materials?

ISO 17034 accreditation offers multiple advantages for

RM purchasers:

• Clear definition for reference material (RM) and

certified reference material (CRM)

• Recognition of the competence of the producer and

its scope

• Strict normative framework – including for the

preparation, homogeneity testing and

characterization

• Regular assessment by an accreditation body

• Guarantee that material is produced according to

technically valid and internationally recognized

principles, and fitted for the intended uses

Conclusion

The quality of your analysis

can never be better

than the quality of

your proofs & standards

Acknowledgements

Quentin Bochud, Christine Stooss, Céline Bärtschi Reference Material Lab

Marco Pisino Group Quality

Aurélien Vigier, Dr. Lynda Si-Ahmed New Business Development Team

Contact us : [email protected]

or during this conference

for any inquiry, help, quote…

Documents

Diapositive 1 - LBMA 2019/6. Reference Materials - Jo… · ISO 17034 Structure General requirements 7.2 Production planning 7.3 Production control 7.4 Material handling and storage