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Laboratory requirements for

ISO/IEC 17025:
accreditation of radon indoor
measurements based on
CR-39 nuclear track detectors
S. Bucci, F.Cioni, S.Gambi, R.Magnanelli,
I.Peroni and G.Pratesi
ARPAT, Enviromental Protection Agency Department of Florence
Tuscany Region
Via Ponte alle Mosse, 211 50144 Florence Italy

24th ICNTS Bologna, 1-5 September 2008


What is ARPAT
Regional Enviromental Agency estabilished since
1996 with 10 Departments (one for each Province
of Tuscany)
Many institutional customers
Monitoring of :Water, Soil and Air quality,
electromagnetic pollution, enviromental noise,
food safety, waste control..
Laboratory of radioactivity : g spectrometry, liquid
scintillation spectrometry..
..Radon measurements

24th ICNTS Bologna, 1-5 September 2008


WHY accreditation
ARPAT performs enviromental monitoring of
many parameters and controls the respect of
legislation limits
This implies the necessity of a good quality of data

Control of laboratory by an independent third


organization provides a guarantee to users (customers)
of the competence and impartiality
of laboratories

24th ICNTS Bologna, 1-5 September 2008


Laboratory Accreditation:
STANDARD ISO/IEC 17025:2005
General requirements for the competence of testing
and calibration laboratories

Accreditation Body provides a guarantee of the competence and


impartiality of laboratories in performance of the accredited tests by
means of periodic technical assessments (assessment visits).

In Italy this function is performed by SINAL (National System for


Accreditation of Laboratories) which assesses and exercises
continuing surveillance over the compliance of the laboratories with
standard ISO/IEC 17025. (Note that several ministerial italian decrees make
reference to ISO/IEC 17025 and SINAL accreditation)
.

24th ICNTS Bologna, 1-5 September 2008


STANDARD ISO/IEC 17025:2005
General requirements for the competence of testing
and calibration laboratories
17025 contains all of the requirements that testing and calibration
laboratories have to meet if they wish to demonstrate that they
operate a management system, are technically competent and are
able to generate technically valid results

The ISO 17025 standard itself is comprised of 5 elements:


1. Scope
2. Normative References
3. Terms and Definitions
4. Management Requirements
5. Technical Requirements
Elements 4 and 5 contain the actual accreditation requirements.
24th ICNTS Bologna, 1-5 September 2008
ISO/IEC 17025 :
Accreditation Requirement

Management Requirements Technical Requirements


(same as ISO 9001)
- Organization - Test and calibration methods and
- Quality system method validation
- Document control - Equipment
- Review of requests, tenders and - Measurement traceability
contracts - Sampling
- Service to client - Handling of test and calibration items
- Complaints - Assuring the quality of test and
- Corrective action calibration results
- Preventive action - Reporting the results
- Control of records
24th ICNTS Bologna, 1-5 September 2008
ARPAT and ISO/IEC 17025
ARPAT has more than 60 laboratory methods since 1998
accredited for chemical, biological and physical enviromental
tests.
Accreditation is granted on the basis of examination of
documentation and the results of assessment visits.
SINAL performs periodic visits in ARPAT (typically 1/year) for
assessment of the technical and organisational requirements.

Our laboratory of radioactivity has 3 accredited methods:


1) 2 g spectrometry on food and milk
2) Radon indoor measurements (2006)

24th ICNTS Bologna, 1-5 September 2008


Technical requirement for accredidation of
radon indoor measurements based on CR-39
nuclear track detectors
Point 5 of ISO/IEC 17025
Many factors determine the correctness and reliability of the test and/or
calibrations performed by a laboratory. These factors include
contribution from:
human factors (5.2)
accomodation and enviromental conditions (5.3)
test and calibration methods and method validation (5.4)
equipment (5.5)
measurement traceability (5.6)
sampling (5.7)
the handling of test and calibration items (5.8)
assuring the quality of test and calibration results (5.9)
reporting the results (5.10)
24th ICNTS Bologna, 1-5 September 2008
Technical requirement for accredidation of
radon indoor measurements based on
CR-39 nuclear track detectors
5.4 Test and calibration methods and method validation
Since standards methods for radon indoor measurements are under
development (11 UNI - Italian National Standards Body,
member of ISO working group) the method ARPAT employed
for radon indoor measurements is a non-standard method (5.4.4)
based on a track analysis system TASL of CR-39 Tastrack detector
chemically etched in a NaOH bath.
In a non-standard method some requirements are to fullfilled and
specially:
- Detailed description of the procedure
- Description of parameters or quantities to be determined
- Detailed description of the procedure for estimating uncertainty

24th ICNTS Bologna, 1-5 September 2008


Technical requirement for accredidation of
radon indoor measurements based on
CR-39 nuclear track detectors
5.4.5 Validation of methods : the confirmation by examination and
the provision of objective evidence that the particular requirements
for a specific use are fullfilled
Determination of the characteristics of the method:
- Calibration using reference standard or reference material
- Comparison of results achieved with other methods
- Interlaboratory comparisons
- systematic assessment of the factors influencing the results
- assessment of uncertainty of the results

24th ICNTS Bologna, 1-5 September 2008


Technical requirement for accredidation of
radon indoor measurements based on
CR-39 nuclear track detectors
16000,0

Calibration : 14000,0

12000,0

Periodic check

Track density (N/cm2)


10000,0

yearly repeated in the same 8000,0

batch or with new batch 6000,0

4000,0

of CR-39 detectors 2000,0

0,0
Exposure at CESNEF Politecnico of Milano 0 1000 2000 3000 4000 5000 6000
Rn Exposition (kBqh/m 3)
7000 8000 9000

Interlaboratory comparison (if you get A) is a track to achieve


laboratory accreditation (not sufficient but necessary)
We partecipate to HPA intercomparison 2007 (A)
24th ICNTS Bologna, 1-5 September 2008
Technical requirement for accredidation of
radon indoor measurements based on
CR-39 nuclear track detectors
(5.4.6) Uncertainty: obtained from the following contributions
- Background counts
- Counting statistics
- Calibration
- Repeatability
Repeatability has been valued by means of different
- chemical etching bath (same temperature and NaOH concentration)
- detectors (within the same batch)
- different microscope scans
14

12

Repeatability of 10
CV %

microscope scans as 6

a function of exposure level 2

0
120 400 2550
Rn exposure (kBqh/m3)

24th ICNTS Bologna, 1-5 September 2008


Technical requirement for accredidation of
radon indoor measurements based on
CR-39 nuclear track detectors
5.5 Equipment : Equipment shall be calibrated or checked before use
Records shall be maintaned of each item of equipment and its
software significant to the test and/or calibration performed
Etching equipment check by means of:
- International standard traceable calibration of the thermal bath thermometer
-Temperature uniformity in the thermal bath
- International standard traceable calibration of hydrometer measuring NaOH solution
density
CR-39 exposed to Am-241

Minimum 2 detectors exposed to 0,25

Am-241 in a fixed configuration 0,2


freqeuncy

0,15

are etched every bath. Control on: 0,1

- number of the tracks 0,05

- morphology of the tracks 0


4 8 12 16 20

diameter (n)
24 28 32 36 40

24th ICNTS Bologna, 1-5 September 2008


Technical requirement for accredidation of
radon indoor measurements based on
CR-39 nuclear track detectors
(5.4.5) Robustness against external influences and/or cross-sensitivity against
interference from the matrix of the sample/test object

Influence of the etching thermal bath time NaOH thermal bath concentration

50,0

Influence of the etching thermal bath NaOH 40,0

concentration 30,0

CV %
20,0

Influence of the etching thermal bath 10,0

temperature 0,0

-10,0
5 5,5 6 6,5 7 7,5

NaOH /N

Influence of the number of detectors in each


thermal bath

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WHAT IS CRITICAL TO GO AHEAD

1. Tracebility of calibration to international reference standards


2. Calculation and data trasnfer subject to appropriate checks
in a systematic manner (i.e. computer software suitably
validated (5.4.7))
(TASL system is not trasparent enough: algorithms to calculate tracks
number are not open source: therefore it is not really possible to keep
under control the process)
3. Technical point: Management of aging and fading
(The two effects are under progressive study, this implies
however long time )

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Conclusions
We showed laboratory requirements for ISO/IEC 17025
accreditation for radon indoor measurements based on CR-39
nuclear track detectors with same pratical examples
Accreditation needs a big effort and human and economical
resources. The wide experience of the Agency on other test
methods helped us very much
However we are convinced that Accreditation is worth while
for two reasons:
The periodic visit of SINAL 1/years allows us to
mantain all the system under control
This stimulates a continuos improvement from a technical
point of view, giving better quality of data and guarantee
to customers
24th ICNTS Bologna, 1-5 September 2008
Extra Sl

Standardization diminishes trade barriers, promotes safety, allows interoperability of products,


systems and services, and promotes common technical understanding.