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Outline for the revision of ISO Guide 35

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DOI: 10.1007/s00769-012-0940-0

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Accred Qual Assur (2013) 18:115–118
DOI 10.1007/s00769-012-0940-0
PRACTITIONER’S REPORT
Outline for the revision of ISO Guide 35
Angelique Botha • Steve Ellison • Thomas Linsinger •
Adriaan van der Veen
Received: 6 September 2012 / Accepted: 15 November 2012 / Published online: 6 December 2012
Ó Springer-Verlag Berlin Heidelberg 2012
Abstract The production of reference materials (RMs) is
a key activity for the improvement and maintenance of a
worldwide coherent measurement system. As detailed in
ISO Guide 33, RMs with different characteristics are used
in measurements, such as calibration, quality control and
method validation, as well as for the assignment of values
to other materials. Currently, ISO Guide 35 is in its third
edition after it was revised in 2006. The Guide was
developed to support best practices in the value assignment
to specified properties of Certified Reference Materials
(CRMs). This Guide gives general guidance and explains
concepts to assist the understanding and development of
valid methods to assign values to the properties of a ref-
erence material, including the evaluation of their associated
measurement uncertainties, and the establishment of their
metrological traceability. From the outcome of a system-
atic review of ISO Guide 35 among the members of ISO/
REMCO, the ISO Committee on Reference Materials, it
followed that there is a need for revising the current edition
Presented at BERM-13, June 2012, Vienna, Austria.
A. Botha (&)
National Metrology Institute of South Africa (NMISA),
CSIR, Building 5, Meiring Naudé Road, Brummeria,
Pretoria 0001, South Africa
e-mail: abotha@nmisa.org
S. Ellison
LGC, Queens Road, Teddington TW11 0LY, UK
T. Linsinger
European Commission, Joint Research Centre,
Institute for Reference Materials and Measurements (IRMM),
Retieseweg 111, 2440 Geel, Belgium
A. van der Veen
VSL, Thijsseweg 11, 2629, JA, Delft, The Netherlands
of ISO Guide 35. The mandate for the revision is focused
on editorial updates to explain the concepts in more detail.
It is not envisaged that major technical changes will be
introduced. This paper explains the approach and rationale
for the revision of ISO Guide 35 and invites comments
from the users of the current edition of ISO Guide 35.
Keywords ISO Guide 35
Reference materials

Value assignment
Homogeneity
Stability
Introduction and background
The production of reference materials (RMs) is a key
activity for the improvement and maintenance of a
worldwide coherent measurement system. As detailed in
ISO Guide 33 [1], RMs with different characteristics are
used in measurements, such as calibration, quality control
and method validation, as well as for the assignment of
values to other materials. Certified reference materials
(CRMs) are also used to confirm or establish metrological
traceability to conventional scales, such as the octane
number, hardness scales and pH. Furthermore, selected
pure substances are used to maintain the international
temperature scale.
To be comparable across borders and over time, mea-
surements need to be traceable to appropriate and stated
references. CRMs play a key role in implementing the
concept of traceability of measurement results in chemis-
try, biology and physics among other sciences dealing with
materials and/or samples. Laboratories use these CRMs as
readily accessible measurement standards to establish
traceability of their measurement results to international
standards. The property values carried by a CRM can be
made traceable to SI units or other internationally agreed
123
116
references during production. ISO Guide 35 explains how
methods can be developed that will lead to well-established
property values, which are made traceable to appropriate
stated references.
For reference material producers (RMPs), there are three
ISO Guides that specifically assist with the set-up of a
scheme to produce and certify RMs to ensure that their
quality meets the requirements of the end-users. ISO Guide
34 [2] outlines the requirements to be met by an RMP to
demonstrate competence. ISO Guide 35 [3] provides gen-
eral guidance on property assessment issues and explains
the concepts for processes such as the assessment of
homogeneity, stability and value assignment for the certi-
fication of RMs. ISO Guide 31 [4] describes the format and
contents of certificates for CRMs and accompanying doc-
uments for other RMs, respectively. ISO Guides 34 and 35
are widely used by RMPs around the globe and have been
translated into several languages, such as Russian, Portu-
guese, Chinese, German and Japanese.
The 3rd edition of ISO Guide 35 has received wide-
spread recognition among the RMPs, the laboratory
community, national metrology institutes and accreditation
bodies. The document is thought to be a companion to ISO
Guide 34 [2] that provides the criteria to be met to show
competence in reference material production. Most
organisations implement ISO Guide 35 alongside ISO
Guide 34.
From the feedback received during the systematic
review of ISO Guide 35, it was seen that in some cases,
ISO Guide 35 is used in the same fashion as ISO Guide 34
by some accreditation bodies. Such use has never been
intended for ISO Guide 35 and is also discouraged in the
scope of the document. It is impossible to detail exactly
how specific clauses of ISO Guide 34 should be imple-
mented in organisations having an operational quality
system. In fact, it can in some aspects be different for every
CRM produced.
Since the release of ISO Guide 35 in 2006, the revised
version of ISO Guide 34 was published. This revision
contains more specificity with respect to requirements for
RMPs, which, in turn, allows for streamlining ISO Guide
35 in its next version. The principles and methods required
for the value assignment to a property of a reference
material, such as the assessment of stability and homoge-
neity need refinement. The role of the statistics in ISO
Guide 35 is also still under debate. Although approaches
contained in ISO Guide 35 for assessing, for example,
between–bottle homogeneity [5], stability [6, 7, 8] can be
applied for a wide variety of reference materials, they
cannot address every single case. This consideration needs
to be more apparent in the revised document, so that it is
clear to the readership that the approaches described are not
meant to be restrictive.
123
Accred Qual Assur (2013) 18:115–118
Proposed new scope for ISO Guide 35
This Guide gives general guidance and explains concepts
to assist with the understanding and development of valid
methods to assign values to the properties of a reference
material, including the evaluation of their associated
measurement uncertainty, and the establishment of their
metrological traceability.
The Guide will be improved in structuring the normative
(‘mandatory’) and informative (‘optional’) material. More
examples of good practice will be added. This Guide
complements ISO Guide 34 by providing detailed
descriptions of acceptable approaches for the production of
reference materials with reference to the assessment of
homogeneity and stability, the characterisation of reference
materials, estimating uncertainties of the assigned values
and by giving information on how to achieve and demon-
strate the metrological traceability of assigned values.
Assessment of homogeneity
Most RMs are prepared as batches of ‘units’ (e.g. bottles,
vials or test pieces). It is important that the material within
each unit is uniform and that all distributed units are the
same within the stated uncertainty for each property.
Accordingly, ISO Guide 34 requires assessment of the
homogeneity of a reference material.
Homogeneity may refer either to variation between
separate units of the material, or to variation within each
unit. It is always necessary to assess the between-unit
variation. Where the intended use permits the use of part of
a unit—for example, a small portion of a solid or liquid
material—it is usually additionally necessary either to
assess the within-unit variability or to provide instructions
for use that control the impact of within-unit variability.
These instructions may include, for example, remixing of
the sample and, for granular materials, a minimum sample
intake.
Assessment of homogeneity may include the use of prior
evidence, the conduct of an experimental homogeneity
study on the candidate reference material, or both. In most
cases, an experimental study is necessary. Exceptions
include, for example, preparations of batches of a highly
homogeneous material such as a solution for which pre-
vious experimental studies have demonstrated that
packaging does not affect homogeneity; or the preparation
of materials for which each reference material unit has a
separate assigned value.
The results of the homogeneity assessment are normally
included in the uncertainty budget of the certified property
value. The magnitude of this uncertainty component can
vary widely compared to other components of the
Accred Qual Assur (2013) 18:115–118
uncertainty, depending on the nature of the RM and of the
certified property.
The descriptions of the assessment of within–bottle and
between–bottle homogeneity will be further refined, with
improved approaches to data evaluation as well as more
details related to selecting test items from the batch. The
current description of taking, at random, an appropriate
number of items [3] has been interpreted by some that
stratified random sampling is not permitted. The nature of
this erroneous conclusion is an example of the kind of
restrictive interpretation that will be corrected in the
revised Guide.
Assessment of stability
Stability of the properties of interest is one of the key
features of any RM. As with assessing homogeneity, a
further refinement of the material currently contained
in ISO Guide 35 is necessary to more fully describe
the considerable progress that has been made since the
introduction of stability testing in reference material
production.
Stability testing of candidate RMs is performed over a
period of time so that the behaviour of the properties of the
material is known. The stability of some physical property
RMs can improve over time. However, for chemical
composition RMs, it is usually true that the stability of
these properties will not improve over time, but may get
worse over time, for example due to the degradation of the
matrix.
Approaches to stability testing can be widely different.
The simplest approach is to take two measurements at
different points in time and to draw conclusions about the
stability over the elapsed time. Other approaches include a
multi-point approach, which enables the reference material
producer to draw conclusions over shorter periods than the
time elapsed between the first and last measurement in the
stability study.
Characterisation of the material
The goal of the characterisation is to determine the
expected value of the property values of a material, which
should be a good estimate of the true value. The expected
value may be the same for many individual units (batch
production), or an individual value may be assigned to each
unit. As described in ISO Guide 34 clause 5.15, charac-
terisation can be achieved by using one or several methods
in one or several laboratories. Special cases of these
approaches are value assignment by gravimetric prepara-
tion and assignment of purity values.
117
Whatever the approach chosen, it shall be ensured that
the metrological traceability of the assigned values is
clearly defined and that only values traceable to the same
metrological reference are combined. In an ideal case, the
International System of Units (SI) acts as that metrological
reference. Many property values are operationally defined;
in these cases, it is additionally necessary to ensure that the
method used is widely accepted and described in sufficient
detail to permit accurate reproduction. Metrological trace-
ability also applies to operationally defined quantities; it
remains essential to ensure traceability to defined metro-
logical references by proper calibration.
Evaluating measurement uncertainty
The uncertainty associated with the assigned value should
be valid for the unit as obtained by a particular user, after
storage at the producer and transport to the user.
The theme is central and key to all activities associated
with the establishment of the property values and their
associated uncertainties. Since the publication of ISO
Guide 35, two supplements to the Guide to the expression
of uncertainty in measurement (GUM) [9] have been
published, one on Monte Carlo methods (Supplement #1
[10]) and one on measurement models with more than one
output quantity (Supplement #2 [11]). Appropriate links to
these documents will be established in ISO Guide 35, so
that the readership is directed, as appropriate, to the GUM
and its supplements.
Evaluation of the uncertainties of the certified values is
mainly a technical task, which is supported by statistical
analysis. No general approach to the evaluation of uncer-
tainty is applicable for all measurement methods and
materials. While the procedures presented in this Guide
apply in the majority of cases, alternatives may be used if
sufficiently justified on technical grounds.
In the evaluation of uncertainties, realistic values should
be obtained through the examination of all significant
sources of uncertainty. The evaluated uncertainty shall be
valid for the complete period of validity of the certificate
issued to the user of the material. For materials whose
values change over time, this change should either be
reflected in the uncertainty or in a time-dependent assigned
value, where the uncertainty of this change is included in
the assigned uncertainty.
Concluding remarks
The new revision of ISO Guide 35 will provide general
guidance for the assignment of property values of reference
materials. The content of the new guide will focus on four
123
118
aspects, that is, the assessment of homogeneity and sta-
bility, the characterisation of the property values and the
estimation of the uncertainty of the certified values. For
batch certification, the assessment of the homogeneity for a
property value of the material should give evidence that the
value is the same within a unit and between different units
within the evaluated uncertainty of the certified value. The
same principle applies to the assessment of stability. It is
important that the certified property values stay the same
within the stated uncertainty at least for the period of
validity of the certificate of the CRM.
In the new edition of ISO Guide 35, the clause on the
characterisation will give more specific guidance on two
methods that are used widely, that is, characterisation using
an interlaboratory comparison study as well as using a
single method in one laboratory. It will especially focus on
the set-up and evaluation of such interlaboratory compar-
ison studies and explain that the certified value must be
obtained by the combination of results of demonstrated
metrological traceability obtained by laboratories of dem-
onstrated competence.
As is the case in the current edition of Guide 35, the new
Guide will be very brief on the preparation/processing
(drying, milling, bottling etc.). This is not because these
processes are not important, but because each material
requires a specific approach and general guidelines are
difficult to provide.
Notice
Working Group 16 of ISO/REMCO welcomes comments
on the proposed outline for the revision of ISO Guide 35, as
described above, and information on practical experience
of using the present edition of ISO Guide 35. Comments
123
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Accred Qual Assur (2013) 18:115–118
can be sent to the convenor, Dr. Angelique Botha
(abotha@nmisa.org).
References
1. ISO Guide 33 (2000) Uses of certified reference materials.
International Organization for Standardization (ISO), Geneva,
p 23
2. ISO Guide 34 (2009) General Requirements for the Competence
of Reference Material Producers. International Organization for
Standardization (ISO), Geneva, p 33
3. ISO Guide 35 (2006) Reference materials—general and statistical
principles of certification. International Organization for Stan-
dardization (ISO), Geneva, p 64
4. ISO Guide 31 (2000) Reference materials—contents of certifi-
cates and labels. International Organization for Standardization
(ISO), Geneva, p 7
5. Van der Veen AMH, Linsinger TPJ, Pauwels J (2001) Uncer-
tainty calculations in the certification of reference materials. 2.
Homogeneity study. Accred Qual Assur 6:26–30
6. Linsinger TPJ, Pauwels J, Van der Veen AMH, Schimmel H,
Lamberty A (2001) Homogeneity and stability of reference
materials. Accred Qual Assur 6:20–25
7. Linsinger TPJ, Pauwels J, Lamberty A, Schimmel HG, Van der
Veen AMH, Siekmann L (2001) Estimating the uncertainty of
stability for matrix CRMs. Fresenius J Anal Chem 370:183–188
8. Lamberty A, Schimmel H, Pauwels J (1997) The study of the
stability of reference materials by isochronous measurements.
Fresenius J Anal Chemistry 360:359–361
9. ISO GUIDE 98-3 (2008) Evaluation of measurement data—guide
to the expression of uncertainty in measurement. International
Organization for Standardization (ISO), Geneva, p 120
10. ISO GUIDE 98-3/Supplement 1 (2008) Evaluation of measure-
ment data—Supplement 1 to the Guide to the expression of
uncertainty in measurement—Propagation of distributions using a
Monte Carlo method. International Organization for Standardi-
zation (ISO), Geneva, p 82
11. ISO GUIDE 98-3/Supplement 2 (2011) Evaluation of measurement
data—Supplement 2 to the Guide to the expression of uncertainty in
measurement—Extension to any number of output quantities.
International Organization for Standardization (ISO), Geneva, p 72