Professional Documents
Culture Documents
OF TESTING LABORATORIES
Jukka Häyrynen
Heikki Kallio
Anna-Maija Kosonen
NORDTEST
Tasks
The tasks of Nordtest are to promote the safety of life, health, environment and material
values and to encourage a free exchange to trade. The approach adopted by Nordtest to
achieve its objectives is:
- to develop, adopt and recommend test methods and to promote the use of these
by industry and the authorities and also in the standardisation work
- to obtain international recognition of test results and also the competence of the
Nordic countries, for instance by quality assurance and verification of testing
activity
- to endeavour that tests and approval of test results are made in a resource and
cost effective manner
Organisation
The organisation consists of a board, a secretariat and nine technical groups. These groups
are Acoustics and Noise, Building, Electronics, Environment, Fire, Mechanics, Polymers, VVS
(Mechanical Building Services) and Quality Assurance.
The work is directed by the board which comprises representatives of all the Nordic
countries, The members are appointed by the government or appropriate department of the
country concerned.
The technical groups initiate and evaluate projects. The projects are often structured in such
a way that they can be used as catalysist for development of the combined technical
competence in the Nordic countries. At present, about 250 Nordic projects are being carried
out in some 40 firms and institutions.
The board as well as the technicai groups are assisted by the secretariat which is responsible
for day to day activity. The secretariat is located at Esbo, Finland.
Financial framework
The cost of the Nordtest secretariat and a Iarge proportion of project activity is financed
from the budget of the Nordic Council of Ministers. The grant for 1992 is approx. 2 millions
ECU, The work of the board and the technical groups is financed by the participating
organisations.
Publications
- Register of 1300 test methods and technical reports
- Test methods
- Technical reports
NT TECHN REPORT 177
Approved 1992-04
Title (English): -
This paper is the final report of NORDTEST Project 956-90-l “Referensmaterial vid
laboratories). The scope of this project was to collect information for the users of reference
materials in the Nordic countries and to propose recommendations for the use of reference
materials
Class (UDC): 620.1 Key words: reference materials, quality assurance, testing
laboratories
1 INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.1 Definitions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
1.2 Certification of reference materials . . . . . . . . . . . . . . . . . . . . . . 7
1.3 Organizations within the CRM schemes . . . . . . . . . . . . . . . . . . 7
6 COMAR DATABASE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
8 CONCLUSIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
1 INTRODUCTION
Reference materials (RMs) are used in various fields of testing to provide users
with accurate reference values and traceability for their measurements, to quantify
and to calibrate methods and equipment and to monitor the performance of the
laboratory. These tests can be complex, or the result is qualitative or is not readily
traceable to national or international standards. A reference material is by defini-
tion a material or substance one or more properties of which are sufficiently well
established to be used for calibration of an apparatus, assessment of a measure-
ment method, or for assigning values to materials1.
RMs are widely used within the field of analytical chemistry, where they form the
basis for ensuring accuracy and for adhering to valid measurement systems. The
use of reference materials is gaining momentum in other fields of testing, too.
1
definition, ISO GUIDE 35
-4-
1.1 Definitions
There are a number of terms often used when dealing with quality assurance of
testing as well as with calibration of equipment and instruments. The definitions
below are collected from various standards to clarify further discussions in the
paper.
WORKING STANDARD
* Reasonably homogeneous, previously analyzed materials, pure com-
pounds, solutions of pure elements etc. used instead of CRMs for fre-
quent checks and in situations when cost or availability limit the use of
CRMs.2
2
Distinction between RMs and working standards is somewhat vague; one
way could be: RM is commercially available whereas a working standard
is manufactured in-house.
-5-
2.1 EN 45001
The EN 45001 standard “General criteria for the operation of testing laboratories”
describing the requirements for the accreditation of laboratories refers to reference
materials as follows:
* The quality manual, and related quality documentation, shall state the
laboratory’s policies and operational procedures established in order to
meet the requirements of this Guide, the quality manual and related
quality documentation shall also contain
...
n) reference to verification practices including interlaboratory
comparisons, proficiency testing programmes, use of reference
materials and internal quality control schemes. (5.2, Quality
system, audit and review)
The ISO 9001 standard “Quality systems. Model for quality assurance in design/
development, production, installation and servicing” describes the requirements for
inspection, measuring and test equipment as follows:
ISO or EN standards on mechanical testing usually have separate standards for the
verification of testing machines. For example hardness and impact testing
machines shall or may be verified by means of standardized blocks (=RMs). This
method is so-called indirect verification (see definitions).
ISO/EN
New EN standards will incorporate corresponding ISO standards and replace the
existing European national standards. These standards contain both direct and
indirect verification methods of testing machines. There are also separate stan-
dards for calibration of standardized blocks to be used for indirect verification of
hardness testing machines.
The hardness values given by the testing machine do not depend only on the
dimensions of the indenter, but also on the surface roughness and the seating of
the indenter. For this reason an indirect verification using RMs is considered
necessary. The indirect verification can be performed with two procedures.
According to the first procedure each hardness scale (Rockwell), different
-12-
hardness ranges and test forces or ball sizes (Brinell) will be verified periodically.
The other possibility is to verify prior to the test only one hardness value that
corresponds approximately to that of the tests to be performed.
ASTM
In ASTM standards instructions for a specific hardness testing method, verifica-
tion of machine and calibration of hardness blocks are in one standard. According
to ASTM standards the direct verification shall be used for new and rebuilt
machines. The indirect method using standardized test blocks may be used in
routine testing to assure the operator that a machine is operating properly.
According to prEN 10 045 Part 2, the main method for verification of impact test
machines is the indirect verification using the Charpy V reference test pieces,
whose breaking energies are known. The dimensional requirements are more
accurate than the requirement for standard test specimens. The test pieces shall be
national test pieces traceable to the BCR test pieces or certified BCR test pieces.
The direct method shall be used, when the machine is being installed or repaired
or if the indirect method gives an incorrect or unacceptable result.
Contrary to the EN standard, the main method in the ISO 442 standard is the
direct verification. The indirect method is not even an alternative to complete
direct verification. The reference test pieces are unnotched and their thickness is
smaller than the standard specimens. The same material shall be tested in parallel
in a reference machine.
The user of a reference material must decide what properties are relevant to the
measurement process. The level (of property value) of the CRM should corre-
spond with the level of the intended measurement. The matrix should be close to
the matrix of the material to be subjected to the measurement process (carbon in
low-alloy steel or carbon in stainless steel). The form should correspond with that
of the intended samples (solid, liquid, gas...). The quantity of the CRM should be
-14-
sufficient; the need to obtain additional CRM during the experimental programme
should be avoided and batches of CRMs should partly overlap in use for continu-
ity. Stability of the CRMs should be ensured or changing of the properties should
be recorded in the certificate. The uncertainty of the certified value should be
acceptable when compared to requirements (legal limits, trade agreements and
commercial requirements, previous experience in the laboratory). Appendix 4
shows an example of a BCR reference material.
Often the availability of certified reference material is limited, the use of the
reference material is extensive or the price of the certified reference material is
high. In these cases the commercial certified reference materials cannot be used
in everyday practice by the laboratories. The laboratories can and are also encour-
aged to produce in-house working standards.
The NIST catalogue gives the following reasons for use of reference
materials:
* To help develop accurate methods of analysis (reference met-
hods);
* To calibrate measurement systems used to:
(a) facilitate exchange of goods,
(b) institute quality control,
(c) determine performance characteristics, or
(d) measure a property at the state-of-the-art limit; and
* To assure the long-term adequacy and integrity of measure-
ment quality assurance programmes.
-16-
Often the standards that define indirect verification of test instruments require the
use of certified reference materials (CRMs) as samples with known levels of the
parameters of interest.
A reduced level of reliability can be allowed for the reference material; this
depends on the requirements set for the instruments, on the level of uncertainty of
the certified reference material (traceable, verified, calibrated material) and on the
performance of the instrument. The laboratory can manufacture its own working
standard reference materials or use reference materials without a certificate as
long as the laboratory has verified and documented the production and the
-17-
4.1.1 Calibration
Much of the testing is destructive or testing affects the attributes measured; often
adjustment, verification or calibration of the instruments with reference material
(or instruments) is required prior to testing. The possibility to re-test the samples
is thus very unlikely and valuable information is received on performance of the
test process by recording the measurements (of known values of attributes) done
prior to the test.
-18-
The process described above is very open and has to be included in the normal
testing procedures. Another way to receive material for performance control is to
include blind samples in the testing process. The open process has the possibility
of biased or specially “good” practice in testing as the CRMs are naturally
identified; blind testing can be difficult to organize and in time samples of known
values of attributes are identified by the personnel. Often it is advisable to
incorporate not only testing but also sample preparation in the blind testing
programmes.
An integral part of successful control is good planning of the sampling and testing
plan along with the number of tests, levels and intervals. Control charts measure
the process over time. There are many ways to draw up these charts; below two
choices are described.
4.2.1 X - R charts
This test tells only if the process is under control, not if the measurements are
within required tolerances. The tolerance limits have to be added to the graphs to
justify evaluation on whether the results are within specifications.
-19-
X-bar
8 LCL
6
4
2
0
R
2.5 | UCL
Fig. 1 X-R chart of a process showing both upper and lower control
limits set at three standard deviations from the average value
lines. Sample lot size is 5 per data point.
A simpler and probably more used method within testing is recording individual
measurements of the attributes of known value i.e. testing CRMs. Fig. 2 shows a
hypothetical chart of this kind. A test is done each morning using a CRM of
known level and uncertainty according to procedures and standards. The graph
shows the uncertainty of the CRM and the (in-house) specification limits for the
tests.
-20-
VALUE VALUE
12 12
10 10
8 8
6 6
4 4
2 2
0 0
0 20 40 60 80 100 0 20 40 60 80 100
VALUE VALUE .
12 12
10 10
8 8
6 6
4 4
2 2
0 0
0 20 40 60 80 100 0 20 40 60 80 100
Figure 2 c) shows a sudden increase in scatter in the results, which could be due
to a mechanical fault in the instrument. Further analysis of the data in figure 2 d)
shows that when the measurements by two operators are separated, the increase
in scatter is probably due to the test being conducted by an operator less skilful
than the initial operator.
A process has to be under control before the quality of the results can be
managed. Timely recording of testing performance and the process charts provide
-21-
simple practical means of finding the level of control of the operations, the
quality of testing and pinpointing the forthcoming problems possibly causing
quality nonconformance.
Interlaboratory tests can be used to study the reliability of test methods (ISO
5725), performance of testing laboratories (proficiency testing) and to estimate the
uncertainty of laboratory performance. Interlaboratory tests need to have a
relatively high number of participants to yield statistically valid results. Thus such
test programmes can be arranged only at relatively long intervals. Proficiency
testing and estimation of uncertainty of test performance can be carried out
between the interlaboratory test programmes through the use of materials whose
performance (level of parameters, repeatability, reproducibility, long-term stability
etc) has been established in statistically valid comparisons (interlaboratory tests).
The repeatability value (r) defines the value below which the absolute difference
between two single test results obtained under identical (repeatability) conditions
may be expected to lie with a probability of 95%, whereas reproducibility value
(R) gives the equivalent limit value when using the same method and test material
but in different conditions (time of test, equipment, personnel, laboratory)4.
4
definition, ISO 5725
-22-
There is several sources to get certified reference materials. Some of the best
known are the Community Bureau of References, BCR, the National Institute of
Standards and Technology, NIST, Laboratory of the Government Chemist, LGC
and Analytical Quality Control Services, AQCS, which is related with Interna-
tional Atomic Energy Agency, IAEA.
5.1 BCR
For the mechanical tests of metals BCR can supply a reference material for
Charpy impact testing and is planning to certify a CRM for tensile testing
(NIMONIC 75, CRM 425, which is currently available as a creep testing refer-
ence material).
5.2 NIST
The National Institute of Standards and Technology (NIST) offers for sale
primarily NIST Standard Reference Materials (SRM’s). These are well-character-
ized materials produced in quantity to improve measurement science. SRM’s are
certified for specific chemical or physical properties. In their certificates NIST
reports the results of the characterization and indicate the intended use of
material.
NIST has the function to develop, produce, and distribute SRM’s that provide a
basis for comparison of measurements on materials, and that aid in the control of
production processes. To perform this function, the Office of Standard Reference
Materials evaluates the requirement of science, industry, and government for
carefully characterized reference materials, and their production and distribution.
6 COMAR DATABASE
The Reference Material Committee (REMCO) of ISO adapted and started jointly
to develop the French reference material database originated by Service de
Matériaux de Réference at the Laboratoire National d’Essais (LNE). The original
goal was to provide answers to the question “Where can I buy a CRM with the
following properties...?” without the need to consult all the catalogue s of the
many suppliers. (Klich 1991)
The database is quite comprehensive and thus searching for relevant reference
materials can be tedious. Good knowledge and experience of the database and
also the tests performed and CRMs needed is necessary to efficiently use the
database.
The distribution of the test methods and the reference materials used in these
laboratories is presented table 1.
-25-
According to the answers, reference materials are quite widely used in hardness
testing and most of reference materials had some certification; there were 7 supp-
liers. Most of the certificates did not fully correspond with the ISO GUIDE 31-
1981 “Contents of certificates of reference materials”. Some certificates referred
to national standards (DIN, BSI) and national requirements and were thus mainly
intended for local use; certificates were not very clear in general.
The most popular (and generally also the most trusted) hardness reference blocks
come from Staatliches Materialprüfungsamt Nordrhein-Westfalen (MPA-NRW),
whose certificates give good information on the reference blocks and their use.
Calibration (and certification) of these blocks is according to DIN 51303.
The British and the French systems have accredited (or recognized) suppliers of
reference blocks and some of the certificates (most of the new certificates) refer
to the accreditation.
Many laboratories used reference blocks with no certificates; some RMs were
rather old, dating from the 1970’s, so the use of the blocks had obviously not
been very frequent.
-26-
The questionnaire showed that the significance of the use of reference materials
is not very well understood or even identified as a part of quality assurance
activity in a testing laboratory. Availability of reference materials and of general
information on reference materials seems very limited.
8 CONCLUSIONS
The reference materials are an integral part of the quality assurance of testing
laboratories. Test performance between laboratories can be harmonized through
use of certified reference materials, and individual laboratories can continually
follow up their own performance and check the instruments between verifications
and calibrations. Reference materials are used also to calibrate and tune instru-
ments which are difficult or impossible to calibrate with direct methods. RMs are
used as a transfer standard between a high-quality instrument and a working
instrument.
-27-
Related standards
The number and quality of reference materials are increasing, although informa-
tion on them has not been spread so well. The active role of BCR has had a
positive effect on the field; bringing laboratories and RM producers (Appendix 5)
together in collaborative programmes will increase knowledge and interest in the
related questions. All CRMs should be produced in a way which would allow for
international use and distribution, preferably through BCR in Europe.
Certification documents
COMAR database
The COMAR database is an effective and efficient way to find relevant certified
reference materials. The database should be at least nationally available (in France
30 Minitel subscribers are currently connected to COMAR). There are two major
concepts of organizing the use of COMAR nationally; on one hand a national
body (accreditation body, national technical information centre etc) could centrally
be responsible for giving out information on reference materials, on the other
hand national laboratories would know better their own technical field and could
thus better serve testing laboratories. A national solution is, however, necessary
to spread the information to all laboratories needing information on reference
materials.
-29-
REFERENCES
ASTM E 23-88. Standard test methods for notched bar impact testing for metallic
materials.
ISO GUIDE 30:1981 (E), Terms and definitions used in connection with reference
materials
Juran, J.M. 1974. Quality Control Handbook. 3rd ed. New York, McGraw-Hill
Book Company. 1780 p.
-30-
prEN 10 045 Part 2:1990, Metallic materials - Charpy impact test - Part 2:
Verification of the testing machine (pendulum impact)
INTRODUCTION
For some ten years the Community Bureau of Reference (BCR), a department of the Commission of the
European Communities, has provided laboratories with a means of carrying out collaborative measurement
studies in Physical Measurements and Chemical Analysis.
To understand the role of the BCR it is important to remember that common written standards (Norms),
although essential to achieve harmonization of measurements, are not sufficient by themselves to avoid
discrepancies of results.
The principle of this contribution is to bring together some of the most expert laboratories of preferably all the
Member States for intercomparison exercises. Results are discussed with all participants. Discrepancies are
given particular attention to identify their causes. Subsequently, additional measurements are made to verify
that the causes of errors can be eliminated. When necessary several successive intercomparisons are done to
study the effect of the different parameters.
When the major sources of errors are eliminated and agreement is reached on a value which can be considered
as the most accurate in the current state of the art, it is essential to provide a means of maintaining the
consistency between laboratories and of disseminating the accurate value to other laboratories. The instruments
or pieces of equipment used to transfer values are called transfer standards in Applied Metrology and reference
materials in Analytical Chemistry.
The Community Bureau of Reference undertakes the establishment of transfer standards and reference materials
which can be used by any laboratory which wishes to verify its methods and calibrate its instruments.
The uncertainty is by definition the estimate of the range of values within which the true value is most likely
to be. The uncertainties given in this catalogue take into consideration the variations between laboratories and
between methods and care is taken not to underestimate uncertainties. They are given at a confidence level of
95%.
A certified reference material can be used by a laboratory to verify if the method used gives results in agreement
with the certified values. If the result is different the user is immediately warned that he has to look for errors
in his method and to find their causes.
For calibration the reference material is used to assign a value to the indication of his instrument.
The BCR programme welcomes any suggestion from industrial organisations, official laboratories, research
establishments or universities, concerning measurements of practical importance that need to be improved or
for which there is a need for reference materials. Further information on the BCR is available on request.
Report
Each sample is usually delivered with a certificate and a report which contains all the data which formed the
basis for the certification. It also gives details on the methods of measurements that were used, recommen-
dations on the best methods to use, and advice for the use of the material.
Excerpts from BCR REFERENCE MATERIALS CATALOG
Appendix 1 2(2)
The certified reference materials which are made available by the BCR were established in response to a need
to help laboratories to improve their measurements. Except when batches of reference materials are very limited,
the BCR makes no restriction in their availability for these specific uses as described in its catalogue.
The BCR cannot supply quantities of these materials for any other types of uses.
1. Purchase orders for reference materials and requests for information should be addressed to:
or by telexing:
BCR -BRUSSELS
21877 COMEU B
All purchase orders should give: CRM numbers indicated in the catalogue, name of the material and number
of units required.
2. Delivery time: 3-4 weeks maximum after receipt of the purchase order by the BCR.
3. Shipment: prices include handling and normal postage (surface mail, air mail). If airfreight is requested, it
has to be paid by the customer.
4. Terms of payment: the payments shall be made preferably by bank transfer following instructions to be
found in the debit note (or invoice) that the customer will receive after delivery of the samples.
Methods of payments such as credit letter are not acceptable. Prices of reference materials are shown in
the price list attached. Payments are expected within 30 days of receipt of the debit note.
Appendix 2 l(2)
Batch E
CRM 016
IMPACT TOUGHNESS
OF V-NOTCH CHARPY SPECIMENS
(Energy level 120 J Nominal)
A unit comprises 5 specimens which must be broken successively in the machine to verify.
The specimens are packed in protective oil and cleaning must done as recommended.
Appendix 2 2(2)
Specimens should be kept in their original packing until they have to be used.
Special attention is drawn to cleaning, for which vigorous methods should be avoided
(e.g. brushes or ultrasonic). The following is recommended :
PARTICIPATING LABORATORIES
METHODS USED
LEGAL NOTICE
This document was prepared under the sponsorship of the Commission of the European
Communities. Neither the Commission of the European Communities nor any person
acting on its behalf makes any warranty or representation, express or implied, that the
use of any information, material, apparatus, method or process disclosed in this document
does not infringe privately owned rights ; or assumes any liability with respect to the use
of, or for damages resulting from the use of, any information, material, apparatus,
methods or process disclosed in this document.
CERTIFICATION REPORT
The work done to certify this reference material is described in a report which is
available to users free of charge upon request.
Provisional address : rue de la Loi 200, B-1049 Brussels - Phone (32 2) 235.50.14 - Fax (32 2) 235.80.72
Appendix 3 l(1)
082 Larsen, B., NORDTEST Guidelines for development of Quality Manuals for testing laboratories. Helsinki
1987. Nordtest, NT Techn Report 082. 60 p. (in English and Danish)
084 Fahlén, P., Madsen, E., Johansen, M.M., Rautiainen, L., Siitonen, V., Herje, J. & Sandberg, P.I.,
Guidelines for development of Quality Manuals in the field of building physics, heating & ventilation
and adjacent technical areas. Helsinki 1987. Nordtest, NT Techn Report 084. 25 p.
104 Häyrynen, J., Draft NORDTEST guidelines for interlaboratory test comparison, Espoo 1988. Nordtest,
NT Techn Report 104. 95 p.
105 Fremstad, D., Lundgren, B., Olsen. H. & Saarela, K., Guidelines for development of Quality Manuals in
the field of chemical analysis. Espoo 1988. Nordtest, NT Techn Report 105. 32 p.
107 Haglund, M., A check list concerning the cost/benefit of laboratory accreditation. Espoo 1989.
Nordtest, NT Techn Report 107. 18 p. (in Swedish)
107:E Haglund, M., Check-list concerning the advantages, cost and disadvantages of laboratory
accreditation. Espoo 1990, NT Techn Report 107 Engl, Edition 2. 9 p.
118 Häyrynen, J., Interlaboratory testing. Espoo 1989. Nordtest, NT Techn Report 118. 11 p.
119 Quality assurance in testing laboratories, Espoo 1989. Nordtest, NT Techn Report 119. 156 p. (in
Dan/Nor/Swed/Engl)
131 Quality assurance in testing activities. Espoo 1990. Nordtest, NT Techn Report 131. 261 p. (in
Dan/Nor/Swed/Engl)
143 Larsen, J.B., An examination of the costs in establishment and maintenance of an accreditation and
the including quality control system. Espoo 1991. Nordtest, NT Techn Report 143. 106 p.
144 Ploug, H.H., Nordtest practical guidelines for round robin tests. Espoo 1991. Nordtest, NT Techn
Report 144. 28 p.
145 Lindskov Hansen, S., Guidelines for the development of software to be used in test and measuring
laboratories. Espoo 1991. Nordtest, NT Techn Report 145. 46 p.
146 Ohlon, R., About procedures for internal quality audits of testing laboratories. Espoo 1991. Nordtest,
NT Techn Report 146. 39 p.
147 Andersson, H., An introductory study of calibration in testing laboratories. Espoo 1991. Nordtest, NT
Techn Report 147. 30 p.
148 Änkö, S. & Sillanpää, J., Requirements on the personnel and organization of testing laboratories.
Espoo 1991. Nordtest, NT Techn Report 148. 70 p. (in Swedish)
149 Forstén, J., A view on the assessment of the technical competence of testing laboratories. Espoo
1991. Nordtest, NT Techn Report 149. 46 p.
164 Sillanpää, J., Requirements of ISO 9002 for testing and inspection. Espoo 1992. Nordtest, NT Techn
Report 164. 42 p.
165 Baade, S., Interpretation of EN 45 001 for fire testing laboratories, Espoo 1992. Nordtest, NT Techn
Report 165. 25 p.
177 Häyrynen, J., Kallio, H. & Kosonen, A.-M., Reference materials in quality assurance of testing
laboratories. Espoo 1992. Nordtest, NT Techn Report 177. 35 p.
178 Änkö, S. Qualification system for the personnel of testing laboratories. Espoo 1992. Nordtest, NT
Techn Report 178. 17 p.
179 Ohlon, R., Comparison of standards with requirements on calibration and testing laboratories, Espoo
1992. Nordtest, NT Techn Report 179. 71 p.
nordtest
Mailing Address: Tekniikantie 12 FIN-02150 Espoo, Finland. Phone +358 9 455 4600, fax +358 9 455 4272
www.nordtest.org