Iaea Al 167

IAEA / AL / 167
Report
IAEA-CU-2006-05 proficiency test on the
Determination of 137Cs and 210Pb in spiked soil
IAEA-CU-2006-05, Seibersdorf, April 2006

INTERNATIONAL ATOMIC ENERGY AGENCY
AGENCY'S LABORATORIES, A 2444 SEIBERSDORF, AUSTRIA
TEL NO.: + 43 1 2600 28226; FAX NO.: + 43 1 2600 28222; E-MAIL: AQCS@IAEA.ORG
http://www.iaea.org/programmes/aqcs/
Department of Nuclear Sciences and Applications

Physics, Chemistry and Instrumentation Laboratory
Chemistry Unit
IAEA / AL /167
Report on the IAEA-CU-2006-05 proficiency test on the

determination of 137Cs and 210Pb in spiked soil
Abdulghani Shakhashiro, Adelaide Maria Gondin Da Foseca Azeredo,

Umberto Sansone, Chang-Kyu Kim, Gyula Kis-Benedek, Alexander Trinkl, Thomas
Benesch, Renate Schorn
Sándor Tarjan
Hungarian National Food Investigation Institute
(IAEA collaborating Centre)
NFII
Seibersdorf, April 2006
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Contact information
Abdulghani Shakhashiro
IAEA
Department of Nuclear Sciences and Applications
Chemistry Unit, Physics, Chemistry and Instrumentation Laboratory (PCI)
Agency's Laboratories (Seibersdorf and Headquarters)
A-2444 Seibersdorf – Austria
Email: a.shakhashiro@iaea.org
Tel: + 43 1 2600 28226

Fax: + 43 1 2600 28222
http://www.iaea.org/programmes/aqcs/
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CONTENTS
Executive summary .................................................................................................................... 5

Acknowledgement...................................................................................................................... 6
1. Introduction ............................................................................................................................ 7
2. Proficiency test objectives...................................................................................................... 8
3. Proficiency test materials ....................................................................................................... 8
3.1 Description of the test samples ........................................................................................ 8
3.2 Spiking procedure for 137Cs and 210Pb in soil.................................................................. 9
3.3 Target values and uncertainties....................................................................................... 9
3.4 Homogeneity of proficiency test samples ...................................................................... 10
4. Performance criteria ............................................................................................................. 12
4.1 Relative bias................................................................................................................... 13
4.2 The Z-score value .......................................................................................................... 13
4.3 The U-score value.......................................................................................................... 13
4.4 Evaluation criteria......................................................................................................... 14
5. Results and discussions ........................................................................................................ 15
6. Conclusions .......................................................................................................................... 15
7. References ............................................................................................................................ 16
List of Appendixes ................................................................................................................... 16
Appendix A: Performance evaluation sorted by radionuclide ................................................. 17
Appendix B: Performance evaluation sorted by laboratory code ............................................ 29
Appendix C: List of participating laboratories ........................................................................ 39
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Executive summary
This report summarises the results of a proficiency test conducted within the frame of the
agreement between the International Atomic Energy Agency and Hungarian National Food
Investigation Institute, as IAEA collaborating Centre in the field of preparation of reference
materials.
This proficiency test was organized and conducted by the Chemistry Unit of the IAEA's
Laboratories located in Seibersdorf (Austria). The soil test material was prepared according to
a validated procedure by the Chemistry Unit staff. Full technical details of the proficiency test
set of materials are described in the report.
40 test samples (reference materials) were distributed to the participating laboratories in
January 2006. The deadline for receiving the results from the participants was set to 20
February 2006. The participating laboratories were requested to analyse the samples
employing the methods used in their routine work, so that their performance on the test
samples could be directly related to the real performance of the laboratory. Each laboratory
was given a confidential code to assure the anonymity of the evaluation results. 8 laboratories
from the 8 initially registered reported to the IAEA their results. The analytical results of the
participating laboratories were compared with the reference values assigned to the reference
materials, and a rating system was applied.
The analytical results of both 137Cs and 210Pb were satisfactory. The analytical uncertainties
associated with the results were, in general, appropriate for the analytes and matrices
considered in the current proficiency test.
With the advent of “mutual recognition” on a world wide basis, it is now essential that
laboratories participate in proficiency testing schemes that will provide an interpretation and
assessment of results which is transparent to the participating laboratory and its “customer”.
New requirements coming into force (ISO/IEC 17025:2005) require that laboratories have to
express their results with the measurement uncertainty. The subject of the evaluation of
measurement uncertainty in analytical laboratories is of relevant interest, and although several
guides have been published analytical scientists frequently regard the process as too
theoretical and not suitable for the estimation of uncertainties of complex techniques. This is
because identifying and quantifying all sources of uncertainty is difficult and laborious for
procedures consisting of numerous steps, many of which are not clearly distinguishable. In
addition, to find objective techniques for deciding the level of uncertainty is acceptable in
measurements intended for particular purposes is a difficult task.
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The following pictures report the analytical data evaluation of this proficiency test. 94 % of
the laboratories reported “acceptable” results for 137Cs and 79 % for 210Pb.
137 210
Cs Pb
Not
Not
Acceptable
Warning Acceptable
8%
3% 3%
Warning
13%
Acceptable
Acceptable 79%
94%
Acknowledgement
The participants and laboratories responded to this proficiency test and contributed their
efforts to the present work are highly appreciated and acknowledged.
The contributions of Mr. Marek Makarewicz from Chemistry Unit, at the Agency’s
Laboratories in Seibersdorf, Austria, are highly appreciated.
We would like to thank also Ms. Karin Will, NAAL PCI secretary, for editing this report.
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1. Introduction
The results of analytical measurements play a vital role in our daily lives. Analytical data may
be the basis upon which economic, legal or environmental management decisions are made,
and they are essential in international trade, environmental protection, safe transportation, law
enforcement, consumer safety and the preservation of human health. As an incorrect decision
can be extremely costly and detrimental, it is essential that such measurements are accurate,
reliable, cost effective and defensible. In addition, measurements performed by laboratories
located worldwide should yield traceable and comparable results.
It is now widely recognised that for a laboratory to produce consistently reliable data it must
implement an appropriate programme of quality assurance measures. Amongst such measures
is the need for the laboratory to demonstrate that its analytical systems are under statistical
control, that it uses methods of analysis that are validated, that its results are “fit-for-purpose”,
and that it participates in proficiency testing exercises [1]. The competence of laboratories is
demonstrated in accreditation processes according to the ISO/IEC 17025:2005 [2] and in the
frame of accreditation systems, the use of reference materials, both for quality control and
proficiency testing, has therefore increased in recent years.
Proficiency testing is a method for regularly assessing the accuracy of the analytical data
produced by the laboratories of particular measurements. In analytical chemistry, proficiency
testing usually comprises the distribution of effectively homogenous portions of the test
material to each participant for analysis as an unknown. The laboratories conduct the test
under routine conditions, and report the result to the organiser by a deadline. The results
generated in proficiency testing should be used for the purpose of a continuing assessment of
the technical competence of the participating laboratories [1]. With the advent of “mutual
recognition” on a world wide basis, it is now essential that laboratories participate in
proficiency testing schemes that will provide an interpretation and assessment of results which
is transparent to the participating laboratory and its “users”. Participation in proficiency
testing exercises provides also laboratories with an objective means of assessing and
documenting the reliability of the data they are producing.
Since the 1960s the International Atomic Energy Agency (IAEA) has played an important
role assisting laboratories in Member States to improve the quality of their analytical results
and their traceability to basic standards. This is accomplished through the provision of matrix
reference materials and validated procedures, training in the implementation of quality
control, and the evaluation of measurement performance by the organization of proficiency
tests and intercomparison exercises. The Chemistry Unit of the IAEA's Laboratories, located
in the vicinity of the village of Seibersdorf (Lower Austria), about 35 km southeast of Vienna,
at the premises of the Austrian Research Centre, is actively involved in the production and
characterization of matrix reference materials of terrestrial origin, widely used for method and
measurement validation and organization of proficiency tests and intercomparison exercises.
The Chemistry Unit is a part of the Physics, Chemistry and Instrumentation Laboratory.
Within the frame of the agreement between the International Atomic Energy Agency and
Hungarian National Food Investigation Institute, as IAEA collaborating Centre in the field of
production and characterisation of matrix reference materials, a proficiency test was organized
and conducted by the Chemistry Unit. The proficiency test was addressed to assess the
analytical performance of 8 laboratories from Hungary on the determination 137Cs and 210Pb in
spiked soil.
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2. Proficiency test objectives
Four distinct aims of the proficiency test can be formulated:

• To check the accuracy and precision of the analytical results produced by the participating
laboratories from Hungary for the determination of 137Cs and 210Pb in spiked soil.
• to encourage the participating laboratories in finding remedial actions where shortcoming
in analytical performance are detected;
• to encourage the use of proper routine quality control measures within individual
laboratories;
• to provide general evaluation and comments on the overall performance of participating
laboratories; and in order to enable the laboratories to compare their performances with
those of other laboratories.
3. Proficiency test materials
In the planning-preparation phase of the proficiency test, the technical requirements regarding
the type of matrices, the array of analytes and the concentration levels of the participants were
discussed. The prime consideration in the choice of the material was that it should be as far as
representative of the type of material that is routinely analysed, in respect of composition of
matrix and the concentration range or number of analytes. According to the users
requirements it was agreed to use soil as test samples with gamma-emitting radionuclides
(137Cs, and 210Pb).
The following proficiency test design was applied:
• one soil sample (sample code 03) at low activity. This soil was used to prepare the spiked
test materials (blank soil),
• duplicate spiked soil samples (sample codes 01, 05), activity level of 137Cs is ~ 10 times of
the blank; and for 210Pb is ~ 5 times.
• duplicate spiked soil samples (sample codes 02, 04), activity level of 137Cs and 210Pb are ~
2 times of samples 01 and 05.
The participant received the test set, together with handling instructions and the reporting
forms. The deadline for data return was set to 20th February 2006.
3.1 Description of the test samples
A soil from China was used to prepare a spiked mineral matrix with 137Cs and 210Pb.
Before using the soil for spiking, it was milled and sieved to collect the appropriate fraction at
mesh size less than 0.1mm, and then homogenised.
The matrix of Chinese soil was characterised and a number of samples were pre-screened for
radionuclides prior to spiking. The results have shown that the material is free from man-
made radionuclides, except for 137Cs, which was present at 2.6 ± 0.2 Bq/kg based on dry
weight (d.w.). (Ref. date: 2006-01-01) and 210Pb at 48 ± 1.5 Bq/kg d.w. The moisture content
determined at 105°C was found to be 2.3 ± 0.2%.
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3.2 Spiking procedure for 137Cs and 210Pb in soil
An aliquot (0.5136g) of the spiking solution was introduced into polypropylene containers
and diluted with 80 ml of methanol. A portion of Chinese soil (para. 3.1) was weighed to the
second decimal place and transferred to the jar containing the spiking solution. The liquid-to-
solid ratio was determined experimentally such that the whole amount of liquid was absorbed
by the soil and the whole amount of soil became uniformly moistened.
The samples were kept in an oven at 40°C for 12 hours to become completely dry. They were
then allowed to reach equilibrium with ambient humidity before sealing. After such treatment
the residual moisture content was found to be 2.4 ± 0.2%, i.e. not very different from the
initial humidity of the untreated sample (2.3 ± 0.2%).
To control the quality of the spiked samples, all of the produced samples were measured by
gamma spectrometry and checked for consistency.
3.3 Target values and uncertainties
The target values were calculated from the certified activity values assigned to each
radionuclide, taking into account the successive dilution steps, the mass of spiking solutions
and the amount of matrix being spiked. The target values for 137Cs and 210Pb in the four
prepared samples together with the respective uncertainties are presented in Tables 1 and 2.
The combined standard uncertainty includes three major components: uncertainty of spiking
solution, uncertainty originated from heterogeneity and one arising from variability of
moisture content in samples. The two latter sources are the largest contributors to the overall
uncertainties which are, nevertheless, gratifyingly small for all radionuclides used in the PT.
Summary of the target values and associated total uncertainties of the test samples are
presented in table 3.
Table 1: Target activities and associated uncertainties of samples 01 and 05
(Reference date: 1 January 2006)
Radio- Activity u(A) u(homogeneity) Dry u(DW) Sample u Sample Activity Combined
nuclide (A) weight mass Mass in soil uncertainty
Bq/sample Bq/sample % Bq/sample % % g Bq*kg-1 d.w. %
137
Cs 3.968 0.056 1.42% 0.078 2.00% 97.7% 0.25% 200.00 0.101 20.3 0.50 2.47%
210
Pb 56.526 0.750 1.33% 1.131 2.00% 97.7% 0.25% 200.00 0.101 289.2 6.98 2.41%
Table 2: Target activities and associated uncertainties of samples 02 and 04

(Reference date: 1 January 2006)
Radio- Activity u(A) u(homogeneity) Dry u(DW) Sample u Sample Activity Combined
nuclide (A) weight mass Mass in soil uncertainty
Bq/sample Bq/sample % Bq/sample % % g Bq*kg-1 d.w. %
137
Cs 7.509 0.114 1.53% 0.113 1.50% 97.7% 0.25% 200.00 0.101 38.4 0.83 2.15%
210
Pb 103.668 1.544 1.49% 1.555 1.50% 97.7% 0.25% 200.00 0.101 530.5 11.3 2.13%
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Table 3: Summary of the target values and associated total uncertainties of the proficiency test
samples
Target value (Bq*kg-1) dw
Sample code
137
Cs 210
Pb
01 , 05 20.3±0.5 289±7
02 , 04 38.4±0.8 530±11
03 2.6±0.2 48.0±1.5
The uncertainty is expressed as 1 σ (k=1), dw = based on dry weight
3.4 Homogeneity of proficiency test samples
The method of spiking soil samples was developed in the Agency's Laboratories in
Seibersdorf and was demonstrated to yield reliable and reproducible results within 1-2% for
all radionuclides tested.
In one series of experiments, a homogeneity test was performed on three bottles of spiked
samples, by measuring 137Cs and 210Pb in 3 sub-samples at a sample mass of 60g taken from
each of the three bottles. The measurements were performed by gamma-spectrometry in the
IAEA Laboratories Seibersdorf [3]. The results were evaluated by single factor ANOVA [6].
It can be concluded that the homogeneity of the material is fitting for the purpose of this
proficiency test. The homogeneity test results are shown in Table 4.
Homogeneity test results provide experimental evidence that satisfactory within-bottle
homogeneity has been attained for both radionuclides for sub-samples weighing 60 g or more.
Table 4: Homogeneity test measurements
Sample ID 210
Pb 137
Cs
R (cps) u(R)/R R (cps) u(R)/R
133-1 6.09E-02 3.5% 6.96E-02 2.0%
133-2 6.28E-02 3.4% 6.79E-02 2.1%
133-3 6.27E-02 3.1% 6.84E-02 2.1%
244-1 6.16E-02 3.5% 7.14E-0 2.1%
244-2 5.93E-02 3.5% 7.03E-02 2.0%
244-5 6.41E-02 2.1% 6.93E-02 2.1%
325-1 5.92E-02 3.5% 7.33E-02 2.0%
325-2 6.22E-02 1.1% 7.05E-02 1.0%
325-3 6.25E-02 3.4% 6.98E-02 2.1%
Average 6.17E-02 7.01E-02
STDV 0.0016 0.0016
Rel. STDV 2.7% 2.3%
To check if there is any trend in the activity values during the spiking procedure, a graphical
evaluation is presented in figures 1 and 2. The slope of the linear fitting was calculated and
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found to be negligible, which illustrates that there is no significant trend on the activity values
of the studied radionuclides during the whole process of spiking.
A second experiment was designed to check if there are any losses of the radionuclides due to
adsorption on the walls of the bottles in which the samples were spiked. Two empty bottles
which have already used in spiking the soil were measured in a gamma-spectrometer. No
activity was detected upon a 24 hour counting. It is therefore concluded that the whole amount
of radionuclides was associated with the matrix.
A second experiment was designed to check if there were any losses of the radionuclides due
to adsorption on the walls of the bottles in which the samples were spiked. Two empty bottles
which have already used to spike the soil were measured by gamma-spectrometer. No activity
was detected upon a 24 hour counting. It is therefore concluded that the whole amount of
radionuclides was associated with the matrix.
There was not need to check the between bottle homogeneity, since each bottle was spiked
individually with the same amount of radionuclides and then each bottle was also individually
homogenised. Therefore, the value of between bottle heterogeneity uncertainty is limited to
the weighing uncertainty and it was estimated that combined uncertainties arising from
heterogeneity is less than 2% and it was included in the total uncertainty budget.
Figure 1: Trend evaluation of the spiking procedure of 210Pb

210
Pb
y = -0.0004x + 0.1871
2.75E-01
2.25E-01
CPS
1.75E-01
1.25E-01
7.50E-02
2 6 12 18 28 34
Bottle num ber
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Figure 2: Trend evaluation of the spiking procedure of 137Cs
137
Cs
y = 0.0003x + 0.0518
1.0E-01
8.0E-02
6.0E-02
CPS
4.0E-02
2.0E-02
0.0E+00
2 6 12 18 28 34
Bottle number
4. Performance criteria
Currently most of laboratories produce test results accompanied, at best, with an indication of
their repeatability only and provide no indication of their analytical uncertainty. However,
new requirements coming into force (ISO/IEC 17025:2005) [2] require that laboratories have
to express their measurement uncertainty.
Several rating systems have been developed for determining a laboratory’s performance and
the meaning of the results of the different scoring systems are not always comparable. Among
various statistics, Z-scores and U-scores are most often used. The drawback of Z-scores is that
uncertainty of the participant’s measurement result is not taken into account for the evaluation
of performance. In the case of U-scores, the evaluation includes uncertainties of the
participant measurements and the uncertainty of the assigned value. Laboratories performing
well in classical proficiency testing (Z-Scores) will not necessarily exhibit the same level of
performance when their analytical uncertainties are considered in the evaluation.
The proficiency testing scoring system applied by the Chemistry Unit in the Agency’s
laboratories takes into consideration the trueness and the precision of the reported data and it
includes in the evaluation both the total combined uncertainty associated with the target value
of proficiency testing samples and the total uncertainty reported by the participating
laboratories. According to the newly adopted approach, the reported results are evaluated
against the acceptance criteria for accuracy and precision and assigned the status “acceptable”
or “not acceptable” accordingly. A result must pass both criteria to be assigned the final status
of “Acceptable”. The advantage of this approach that it checks the credibility of uncertainty
statement given by the participating laboratories, and results are no longer compared against
fixed criteria but participants establish their individual acceptance range on the basis of the
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uncertainties assigned to the values. Such an approach highlights not only methodological
problems affecting accuracy of the reported data but also identifies shortcomings in
uncertainty estimation.
In addition, other three statistical parameters namely: Z-score, IAEA/Laboratory result ratio
and relative bias are calculated as complementary information for the participating
laboratories.
4.1 Relative bias
The first stage in producing a score for a result ValueAnalyst (a single measurement of analyte
concentration in a test material) is obtaining the estimate of the bias. To evaluate the bias of
the reported results, the relative bias between the Analyst’s value and the IAEA value is
calculated and expressed as a percentage:
Value Analyst − Value IAEA

Re lative bias = × 100% (1)
Value IAEA
4.2 The Z-score value
The Z-score is calculated from the laboratory results, the assigned value and a standard
deviation in accordance to the following equation:
Value Analyst − Value IAEA
Z Score = (2)
σ
On the basis of “fitness for purpose” principle, the target value for the standard deviation (σ)
is:
0.10 x ValueIAEA
The laboratory performance is evaluated as satisfactory if | z Score | < 2; questionable for

2<| z Score |<3, and unsatisfactory for | z Score |≥3.
4.3 The U-score value
The value of the Utest score calculated according to the following equation [5]
Value IAEA − Value Analyst

u test = (3)
Unc.2IAEA + Unc.2Analyst
The calculated Utest value is compared with the critical values listed in the t-statistic tables to
determine if the reported result differs significantly from the expected value at a given level of
probability. The advantage of Utest that it takes into consideration the propagation of
measurement uncertainties when defining the normalised error, this is especially useful when
evaluating results, which may overlap with the reference interval.
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It should be noted that the choice of the significance level is subjective. For this proficiency
test we have set the limiting value for the u-test parameter to 2.58 for level of probability at
99% to determine if a result passes the test (u < 2.58).
4.4 Evaluation criteria
The proficiency test results were evaluated against the acceptance criteria for trueness and
precision and assigned the status “Acceptable”, “Warning” or “Not Acceptable” accordingly.
4.4.1 Trueness
The participant result is assigned “Acceptable” status if:
A1 ≤ A2
where:
A1 = Value IAEA − Value Analyst
A2 = 2.58 × Unc IAEA

2
+ Unc Analyst
2
4.4.2 Precision
The participant result is assigned “Acceptable” status if:
 Unc IAEA   Unc Analyst 

2 2
P=   +   × 100%
 Value 
 Value IAEA   Analyst 
The acceptance criterion for precision is dependent on the concentration or activity

concentrations of the considered analytes. Applying the above reported equation the
participant result is assigned “Acceptable” status if P is:
• ≤ 20% for 137Cs
• ≤ 20% for 210Pb
A result must obtain “Acceptable” status in both criteria to be assigned final status of
“Acceptable”. If a result obtained a “Not Acceptable” status for trueness or precision, then
the relative bias is compared to a predetermined limit (20% for 137Cs and 25% for 210Pb), and
if a result bias is below this limit then the status “Warning” is assigned as a final score,
otherwise the status “Not Acceptable” is assigned as a final score. Obviously, if a result
obtained “Not Acceptable” status for both trueness and precision the final score will be
assigned as “Not Acceptable”.
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5. Results and discussions
8 laboratories from the 8 initially registered reported to the IAEA their results. Altogether 80
results were submitted. The participants’ data along with the performance evaluation criteria
and evaluation scores were compiled and presented in tables which constitute an integral part
of this report. Performance evaluation for 137Cs and 210Pb measurements is reported in
Appendix A, while the performance evaluation sorted by laboratory code is presented in
Appendix B.
The performance evaluation results showed that the 137Cs measurements had a higher final
score than those related to 210Pb determination. In general, the analytical uncertainties
associated with the results were appropriate for the analytes and matrices considered in the
current proficiency test.
The results submitted by the laboratories were evaluated against the reference values, the
uncertainties claimed by the laboratories were revised and taken into consideration during the
evaluation and when possible.
6. Conclusions
Within the frame of the agreement between the International Atomic Energy Agency and
Hungarian National Food Investigation Institute, as IAEA collaborating Centre in the field of
preparation of reference materials, a proficiency test was organized and conducted by the
Chemistry Unit of the IAEA's Seibersdorf Laboratories (Austria). This exercise demonstrates
an example of fruitful cooperation between the IAEA and one of its collaborating centres.
Such activity enhances the know-how exchange and mutual cooperation.
40 test samples were distributed by the Chemistry Unit to the participating laboratories in
January 2006. The participating laboratories were requested to analyse the samples employing
the methods used in their routine work, so that their performance on the test samples could be
directly related to assess the real performance of the laboratory. Each laboratory was given a
confidential code to assure the anonymity of the evaluation results. All participating
laboratories reported their results to the IAEA. The analytical results of the participating
laboratories were compared with the reference values assigned to the reference materials and a
rating system was applied for determining the laboratories performance.
The analytical data evaluation of this proficiency test indicates that 94% of the laboratories
reported “acceptable” results for the 137Cs and 79% for 210Pb.
The analytical results were satisfactory for both radionuclides
It is worthy to note that proficiency testing has to be carried out within the context of an
application of a complete system for quality assurance in each laboratory to provide a
participant laboratory with an indication of problems if they are present. It is clear that
successful performance in a proficiency test for one analyte does not indicate that a laboratory
is equally competent in determining an unrelated analyte.
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7. References
1. ISO Guide 34:2000 (E) (2000) General requirements for the competence of reference
material producers. ISO, Geneva, Switzerland
2. ISO/IEC 17025:2005, General Requirements for the Competence of Testing and
Calibration Laboratories, ISO, Geneva.
3. MAKAREWICZ, M., Gamma Analysis report, Chemistry Unit, Agency's Laboratories.
4. Quantifying uncertainties in analytical measurements, Eurachem/Citac Guide, 2000.
5. BROOKES, C.J., BETTELEY, I.G., LOXTON, S.M.; Fundamentals of Mathematics and
Statistics, Wiley 1979.
6. ISO/IEC Guide 35, Certification of reference materials-General and statistical principles,
ISO, Geneva, 2000.
List of Appendixes
Appendix A: Performance evaluation sorted by radionuclide
Appendix B: Performance evaluation sorted by laboratory code
Appendix C: List of participating laboratories
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APPENDIX A: Performance evaluation sorted by
radionuclide
Page 17
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Target value: 20.3
Uncertainty: 0.50
[Bq/kg] Data Evaluation of 137Cs in spiked soil, sample code 01
Laboratories Results Acceptance criteria Final
Lab. Code Value Unc. Trueness Precision Score
Bias(%) Z-Score U-Score Lab./IAEA
[Bq/kg] [Bq/kg] % A1 A2 Score P Score
01 20.10 1.10 5.5% -1.0% -0.10 -0.17 0.99 0.20 3.12 Acceptable 6.0% Acceptable Acceptable
Table legend:
A1: Value IAEA − Value Laboratory

30.0
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
Cs Activity [Bq/Kg]
25.0
 UncIAEA   UncLab 
2 2
P:   +  X100%
 Value   Value 
20.0  IAEA   Lab. 
15.0
137
10.0
01 02 03 04 05 06 07 08
Laboratory Code
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Target value: 289.2
Uncertainty: 6.98
[Bq/kg] Data Evaluation of 210Pb in spiked soil, sample code 01
02 324.70 26.30 8.1% 12.3% 1.23 1.30 1.12 35.45 70.20 Acceptable 8.5% Acceptable Acceptable
08 243.10 16.00 6.6% -16.0% -1.60 -2.64 0.84 46.15 45.04 Not Acceptable 7.0% Acceptable Warning
Table legend:

400.0
375.0 A2: 2 . 58 × Unc 2

IAEA + Unc 2
Laboratory
350.0
Pb Activity [Bq/Kg]
2 2
325.0
P:   +  X100%
300.0  IAEA   Lab. 
275.0
250.0
210
225.0
200.0
01 02 03 04 05 06 07 08
Laboratory Code
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Target value: 38.4
Uncertainty: 0.83
Table legend:

55.0
50.0 A2: 2 . 58 × Unc 2

IAEA + Unc 2
Laboratory
Cs Activity [Bq/kg]
45.0
2 2
   
 Value  +  Value  X100%
40.0 P:
35.0  IAEA   Lab. 
30.0
137
25.0
20.0
01 02 03 04 05 06 07 08
Laboratory Code
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Target value: 530 [Bq/kg]
Uncertainty: 11.3
Data Evaluation of 210Pb in spiked soil, sample code 02
Lab. Code Value Unc. Bias(%) Z-Score U-Score
Laboratory/IAEA Trueness Precision Score
Table legend:
650.0
610.0
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
Pb Activity [Bq/kg]
570.0
2 2
530.0 P:   +  X100%
490.0  IAEA   Lab. 
450.0
210
410.0
370.0
01 02 03 04 05 06 07 08
Laboratory Code
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Target value: 2.62
Uncertainty: 0.20
02 2.70 0.60 22.2% 3.1% 0.31 0.13 1.03 0.08 1.63 Acceptable 23.5% Not Acceptable Warning
05 1.82 0.59 32.6% -30.4% -3.04 -1.27 0.70 0.80 1.62 Acceptable 33.4% Not Acceptable Not Acceptable
Table legend:

5.0
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
4.0
Cs Activity [Bq/Kg]
2 2
3.0 P:   +  X100%
 IAEA   Lab. 
2.0
1.0
137
0.0
01 02 03 04 05 06 07 08
Laboratory Code
Page 23
Target value: 48
Uncertainty: 1.5
Bias(%) Z-Score U-Score Laboratory/IAEA
01 39.00 27.00 69.2% -18.8% -1.88 -0.33 0.81 9.00 69.77 Acceptable 69.3% Not Acceptable Warning
02 102.80 22.10 21.5% 114.2% 11.42 2.47 2.14 54.80 57.15 Acceptable 21.7% Not Acceptable Not Acceptable
03 39.00 27.00 69.2% -18.8% -1.88 -0.33 0.81 9.00 69.77 Acceptable 69.3% Not Acceptable Warning
08 32.50 8.50 26.2% -32.3% -3.23 -1.80 0.68 15.50 22.27 Acceptable 26.3% Not Acceptable Not Acceptable
Table legend:
120.0
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
100.0
Pb Activity [Bq/Kg]
2 2
P:   +  X100%
80.0
60.0
40.0
210
20.0
0.0
01 02 03 04 05 06 07 08
Laboratory Code
Page 24
24
Target value: 38.4
Uncertainty: 0.83
Table legend:
60
55
50
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
Cs Activity [Bq/kg]
45
2 2
   
 Value  +  Value  X100%
P:
 IAEA 
40
 Lab. 
35
30
137
25
20
01 02 03 04 05 06 07 08
Laboratory Code
Page 25
Target value: 530
Uncertainty: 11.3
Bias(%) Z-Score U-Score Laboratory/IAEA
Table legend:

600
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
550
Pb activity [Bq/kg]
2 2
P:   +  X100%
 IAEA   
500
Lab.
450
210
400
350
01 02 03 04 05 06 07 08
Laboratory Codes
Page 26
26
Target value: 20.3
Uncertainty: 0.50
Table legend:

35.0
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
30.0
Cs Activity [Bq/kg]
2 2
25.0 P:   +  X100%
20.0
15.0
137
10.0
01 02 03 04 05 06 07 08
Laboratory Code
Page 27
Target value: 289.2
Uncertainty: 6.98
08 220.40 14.10 6.4% -23.8% -2.38 -4.38 0.76 68.85 40.59 Not Acceptable 6.8% Acceptable Not Acceptable
Table legend:

425
A2: 2 . 58 × Unc 2
IAEA + Unc 2
Laboratory
375
Pb Activity [Bq/kg]
2 2
P:   +  X100%
325  Value   Value 
275
210
225
175
01 02 03 04 05 06 07 08
Laboratory Code
Page 28
28
APPENDIX B: Performance evaluation sorted by
laboratory code
Page 29
Page 30
30
Analytical Performance Evaluation of Laboratory 01
137
Cs and 210Pb in spiked soil
Reference date: 1 - 01- 2006

IAEA Laboratory Acceptance criteria
Sample
Analyte Value Unc. Value Unc. R. bias Z-score U-Test Lab./IAEA Trueness Precision Final score
code
[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score
137
Cs 01 20.3 0.50 20.10 1.10 5.5% -1% -0.10 -0.17 0.99 0.20 3.12 Acceptable 6.0% Acceptable Acceptable
Pb 01 289.2 6.98 260.00 37.00 14.2% -10% -1.01 -0.78 0.90 29.25 97.15 14.4%
210
Acceptable Acceptable Acceptable
137
Cs 02 38.4 0.83 39.50 2.10 5.3% 3% 0.29 0.49 1.03 1.10 5.83 Acceptable 5.7% Acceptable Acceptable
Pb
210
02 530.0 11.3 525.0 57.0 10.9% -1% -0.09 -0.09 0.99 5.00 149.92 Acceptable 11.1% Acceptable Acceptable
Cs 03 2.6 0.20 2.54 0.25 9.8% -3% -0.31 -0.25 0.97 0.08 0.83 12.5%
137
Pb
210
03 48.0 1.5 39.0 27.0 69.2% -19% -1.88 -0.33 0.81 9.00 69.77 Acceptable 69.3% Not Acceptable Warning
137
Pb 04 530.0 11.3 482.0 54.0 11.2% -9% -0.91 -0.87 0.91 48.00 142.34 11.4%
210
Cs
137
05 20.3 0.5 22.4 1.2 5.4% 10% 1.03 1.62 1.10 2.10 3.35 Acceptable 5.9% Acceptable Acceptable
Pb
210
Page 31
137

Sample
code
137
Cs 01 20.3 0.50 20.20 1.10 5.4% 0% -0.05 -0.08 1.00 0.10 3.12 Acceptable 6.0% Acceptable Acceptable
Pb
210
137
Pb
210
Cs 03 2.6 0.20 2.70 0.60 22.2% 3% 0.31 0.13 1.03 0.08 1.63 23.5%Not Acceptable
137
Acceptable Warning
Pb
210
03 48.0 1.5 102.8 22.1 21.5% 114% 11.42 2.47 2.14 54.80 57.15 Acceptable 21.7%Not AcceptableNot Acceptable
137
Pb
210
137
Pb
210
Page 32
32
137

Sample
code
137
Pb
210
137
Pb
210
Cs 03 2.6 0.20 2.54 0.25 9.8% -3% -0.31 -0.25 0.97 0.08 0.83 12.5% Acceptable
137
Acceptable Acceptable
Pb
210
03 48.0 1.5 39.0 27.0 69.2% -19% -1.88 -0.33 0.81 9.00 69.77 Acceptable 69.3%Not Acceptable Warning
137
Pb
210
137
Pb
210
Page 33
137

Sample
code
137
Pb
210
137
Pb
210
Cs 03 2.6 0.20 2.50 0.40 16.0% -5% -0.46 -0.27 0.95 0.12 1.15 17.7% Acceptable
137
Acceptable Acceptable
Pb
210
137
Pb
210
137
Pb
210
Page 34
34
137

Sample
code
137
210
Pb 01 289.2 6.98 275.90 20.40 7.4% -5% -0.46 -0.62 0.95 13.35 55.63 Acceptable 7.8% Acceptable Acceptable
137
210
137
Cs 03 2.6 0.20 1.82 0.59 32.6% -30% -3.04 -1.27 0.70 0.80 1.62 Acceptable 33.4% Not Acceptable Not Acceptable
210
Pb 03 48.0 1.5 52.9 8.3 15.6% 10% 1.02 0.58 1.10 4.89 21.68 Acceptable 15.9% Acceptable Acceptable
137
210
137
Pb
210
Page 35
137

Sample
code
Cs 01 20.3 0.50 19.70 0.90 4.6% -3% -0.30 -0.58 0.97 0.60 2.66 5.2%
137
Pb
210
137
Pb
210
137
Pb
210
137
Pb
210
Cs
137
Pb
210
Page 36
36
137 210
Cs and Pb in spiked soil

Sample
code
Cs 01 20.3 0.50 19.60 1.03 5.3% -3% -0.34 -0.61 0.97 0.70 2.95 5.8%
137
Pb 01 289.2 6.98 273.00 12.40 4.5% -6% -0.56 -1.14 0.94 16.25 36.72 5.1%
210
Cs 02 38.4 0.83 39.10 1.72 4.4% 2% 0.18 0.37 1.02 0.70 4.93 4.9%
137
Pb 02 530.0 11.3 500.0 21.0 4.2% -6% -0.57 -1.26 0.94 30.00 61.53 4.7%
210
Cs 03 2.6 0.20 2.26 0.38 16.8% -14% -1.37 -0.84 0.86 0.36 1.11 Acceptable 18.5% Acceptable
137
Acceptable
Pb 03 48.0 1.5 54.1 5.2 9.6% 13% 1.27 1.13 1.13 6.10 13.96 Acceptable 10.1% Acceptable
210
Acceptable
Cs 04 38.4 0.83 38.60 1.72 4.5% 0% 0.05 0.09 1.00 0.18 4.92 4.9%
137
Pb 04 530.0 11.3 504.0 21.5 4.3% -5% -0.49 -1.07 0.95 26.00 62.66 4.8%
210
137
Pb
210
Page 37
137

Sample
code
137
Pb
210
01 289.2 6.98 243.10 16.00 6.6% -16% -1.60 -2.64 0.84 46.15 45.04 Not Acceptable 7.0% Acceptable Warning
137
Pb
210
137
Pb
210
03 48.0 1.5 32.5 8.5 26.2% -32% -3.23 -1.80 0.68 15.50 22.27 Acceptable 26.3%Not Acceptabl Not Acceptable
137
Pb
210
Cs 05 20.3 0.5 18.4 1.0 5.4% -9% -0.94 -1.70 0.91 1.90 2.88 6.0%
137
210
Pb 05 289.2 7.0 220.4 14.1 6.4% -24% -2.38 -4.38 0.76 68.85 40.59 Not Acceptable 6.8% Acceptable Not Acceptable
Page 38
38
Appendix C: List of participating laboratories
Csendes Zsuzsa Animal Health and Food Control Station of

county Baranya
7623 Pécs Megyeri út 24
csendesz@oai.hu
Jáki Istvánné Animal Health and Food Control Station of

county Somogy
7400 Kaposvár Tinódi L.S.u.
i.jaki@axelero.hu
Hetényiné Pap Viktória Animal Health and Food Control Station of

county Bacs-Kiskun
6000 Kecskemét Széchenyi krt. 29.
moricz6@freemail.hu
Kadlátné Vékony Edit Animal Health and Food Control Station of

county Borsod-Abaúj-Zemplén
3534 Miskolc Stadion út 39/a.
bazella@axelero.hu
Kaszás Judit Animal Health and Food Control Station of

county Vas
9700 Szombathely Zanati u. 3.
kaszasj@oai.hu
Molnár Lajos Animal Health and Food Control Station of

county Hajdú-Bihar
4030 Debrecen Diószegi út 30.
molnarl@oai.hu
Nagyné Somogyi Rita Animal Health and Food Control Station of

county Veszprém
8200 Veszprém Mártírok u. 11/a.
Sipos Katalin Animal Health and Food Control Station of

county Heves
3300 Eger Szövetkezet utca 4. Pf. 132.
Sipos.Katalin@oai.hu
Page 39

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IAEA / AL / 167

IAEA-CU-2006-05, Seibersdorf, April 2006

Department of Nuclear Sciences and Applications

Report on the IAEA-CU-2006-05 proficiency test on the

Abdulghani Shakhashiro, Adelaide Maria Gondin Da Foseca Azeredo,

Seibersdorf, April 2006

Tel: + 43 1 2600 28226

Executive summary .................................................................................................................... 5

Four distinct aims of the proficiency test can be formulated:

3. Proficiency test materials

3.1 Description of the test samples

Bq/sample Bq/sample % Bq/sample % % g Bq*kg-1 d.w. %

Table 2: Target activities and associated uncertainties of samples 02 and 04

Bq/sample Bq/sample % Bq/sample % % g Bq*kg-1 d.w. %

The uncertainty is expressed as 1 σ (k=1), dw = based on dry weight

3.4 Homogeneity of proficiency test samples

Figure 1: Trend evaluation of the spiking procedure of 210Pb

4.1 Relative bias

Value Analyst − Value IAEA

4.2 The Z-score value

The laboratory performance is evaluated as satisfactory if | z Score | < 2; questionable for

4.3 The U-score value

Value IAEA − Value Analyst

4.4 Evaluation criteria

The participant result is assigned “Acceptable” status if:

A2 = 2.58 × Unc IAEA

The participant result is assigned “Acceptable” status if:

 Unc IAEA   Unc Analyst 

The acceptance criterion for precision is dependent on the concentration or activity

A1: Value IAEA − Value Laboratory

A1: Value IAEA − Value Laboratory

375.0 A2: 2 . 58 × Unc 2

A1: Value IAEA − Value Laboratory

50.0 A2: 2 . 58 × Unc 2

A1: Value IAEA − Value Laboratory

A1: Value IAEA − Value Laboratory

A1: Value IAEA − Value Laboratory

A1: Value IAEA − Value Laboratory

A1: Value IAEA − Value Laboratory

A1: Value IAEA − Value Laboratory

Reference date: 1 - 01- 2006

Reference date: 1 - 01- 2006

Reference date: 1 - 01- 2006

Reference date: 1 - 01- 2006

Reference date: 1 - 01- 2006

Reference date: 1 - 01- 2006

Reference date: 1 - 01- 2006

Reference date: 1 - 01- 2006

Csendes Zsuzsa Animal Health and Food Control Station of

Jáki Istvánné Animal Health and Food Control Station of

Hetényiné Pap Viktória Animal Health and Food Control Station of

Kadlátné Vékony Edit Animal Health and Food Control Station of

Kaszás Judit Animal Health and Food Control Station of

Molnár Lajos Animal Health and Food Control Station of

Nagyné Somogyi Rita Animal Health and Food Control Station of

Sipos Katalin Animal Health and Food Control Station of

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