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Page 1: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

IAEA / AL / 166ReportIAEA-CU-2006-02 Proficiency Test on the Determination of 137Cs and 210Pb in spiked soilCRP DI.50.08 "Assess the effectiveness of soil conservation measures for sustainable watershed management using fallout radionuclides", Seibersdorf, March 2006

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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: [email protected]

http://www.iaea.org/programmes/aqcs/

Department of Nuclear Sciences and Applications

Physics, Chemistry and Instrumentation Laboratory Chemistry Unit

IAEA / AL /166

Report on the IAEA-CU-2006-02 proficiency test on the

determination of 137Cs and 210Pb in spiked soil Within the frame of CRP DI.50.08

“Assess the effectiveness of soil conservation measures for sustainable watershed management using fallout radionuclides”

Abdulghani Shakhashiro, Adelaide Maria Gondin Da Foseca Azeredo, Umberto Sansone, Chang-Kyu Kim, Gyula Kis-Benedek, Alexander Trinkl, Thomas

Benesch, Renate Schorn

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: [email protected] 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 5.1 General .......................................................................................................................... 15 5.2 Recommendations to the participating laboratories ..................................................... 15

6. Conclusions .......................................................................................................................... 18 7. References ............................................................................................................................ 19 List of Appendixes ................................................................................................................... 19 Appendix A: Performance evaluation sorted by radionuclide ................................................. 21 Appendix B: Performance evaluation sorted by laboratory code ............................................ 33 Appendix C: List of participating laboratories ........................................................................ 49

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Executive summary

This report summarises the results of a proficiency test conducted under the IAEA contract research project CRP DI.50.08 “Assess the effectiveness of soil conservation measures for sustainable watershed management using fallout radionuclides”. It is known that soil erosion undermines agricultural development in two ways. First, it further impoverishes low-income farm households by reducing agricultural yields and incomes. Second, it reduces productivity in irrigated farming systems by contributing suspended sediment to waterways. The costs of these and other effects are substantial in many countries. The fallout radionuclides 210Pb and 137Cs are therefore widely used in soil erosion studies. Consequently it is rather important to assure that the conclusions of soil erosion studies are based on reliable and validated analytical results and to ensure the comparability of the results of different countries. This proficiency test was organized and conducted by the Chemistry Unit of the IAEA's Laboratories located in Seibersdorf (Austria) upon a request from the participants of the CRP. 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. 90 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. 14 laboratories from the 18 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. In the case of 137Cs, the analytical results were satisfactory, while the 210Pb analysis indicated the need for corrective actions in the analysis process. 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 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 how much 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. 82 % of the laboratories reported “acceptable” results for 137Cs and 33 % for 210Pb.

Acknowledgement

The participants and laboratories responded to this proficiency test and contributed their efforts to the present work are highly appreciated and acknowledged. We would like also to thank the IAEA collaborating centre: Hungarian National Food Investigation Centre (NFII), Budapest, Hungary; which contributed time, know how and facilities for milling and testing the homogeneity of the soil used in this proficiency test. The NFII contribution was at no cost to the IAEA. The contributions of Mr. Marek Makarewicz from Chemistry Unit, at the Agency’s Laboratories in Seibersdorf, Austria, are highly appreciated. The assistance of Ms. Karin Will, NAAL PCI secretary, in editing this report is also appreciated.

137 CsWarning13%

Acceptable82%

Not acceptable

5%

210 Pb

Not Acceptable

50%

Acceptable33%

Warning17%

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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 following 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]. 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. In the frame of the IAEA CRP DI.50.08 “Assess the effectiveness of soil conservation measures for sustainable watershed management using fallout radionuclides”, a proficiency test was organized and conducted by the Chemistry Unit. The proficiency test was addressed to assess the analytical performance of 18 laboratories from all over the world, 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 and agreed with the Technical Officer of the IAEA CRP DI.50.08. 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)

Activity (A)

u(A) u(homogeneity) Dry weight

u(DW) Sample mass

u Sample Mass

Activity in soil

Combined uncertainty

Radio-nuclide

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

137Cs 3.968 0.056 1.42% 0.078 2.00% 97.7% 0.25% 200.00 0.101 20.3 0.50 2.47%

210Pb 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)

Activity (A)

u(A) u(homogeneity) Dry weight

u(DW) Sample mass

u Sample Mass

Activity in soil

Combined uncertainty

Radio-nuclide

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

137Cs 7.509 0.114 1.53% 0.113 1.50% 97.7% 0.25% 200.00 0.101 38.4 0.83 2.15%

210Pb 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 137Cs 210Pb

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 [4]. 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

210Pb 137Cs Sample ID R (cps) u(R)/R R (cps) u(R)/R

133-1 133-2 133-3

6.09E-02 6.28E-02 6.27E-02

3.5% 3.4% 3.1%

6.96E-02 6.79E-02 6.84E-02

2.0% 2.1% 2.1%

244-1 244-2 244-5

6.16E-02 5.93E-02 6.41E-02

3.5% 3.5% 2.1%

7.14E-0 7.03E-02 6.93E-02

2.1% 2.0% 2.1%

325-1 325-2 325-3

5.92E-02 6.22E-02 6.25E-02

3.5% 1.1% 3.4%

7.33E-02 7.05E-02 6.98E-02

2.0% 1.0% 2.1%

Average STDV

Rel. STDV 6.17E-02 0.0016 2.7%

7.01E-02 0.0016 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

210Pby = -0.0004x + 0.1871

7.50E-02

1.25E-01

1.75E-01

2.25E-01

2.75E-01

2 6 12 18 28 34

Bottle number

CPS

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Figure 2: Trend evaluation of the spiking procedure of 137Cs

137Csy = 0.0003x + 0.0518

0.0E+00

2.0E-02

4.0E-02

6.0E-02

8.0E-02

1.0E-01

2 6 12 18 28 34Bottle number

CPS

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

ValueValuebiaslativeRe

IAEA

IAEAAnalyst 100×−

= (1) 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:

σ

IAEAAnalystScore

ValueValueZ

−= (2)

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]

22.. AnalystIAEA

AnalystIAEAtest

UncUnc

ValueValueu

+

−= (3)

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:

21 AA ≤ where:

A1 = AnalystIAEA ValueValue −

A2 = 2258.2 AnalystIAEA UncUnc +× 4.4.2 Precision The participant result is assigned “Acceptable” status if:

P = %10022

×

+

Analyst

Analyst

IAEA

IAEAValueUnc

ValueUnc

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 5.1 General 14 laboratories from the 18 initially registered reported to the IAEA their results. Altogether 130 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. The 210Pb analysis indicated the need of corrective actions in the analysis process, to improve the quality of the results. The analytical uncertainties associated with the results were, in general appropriate, for the analytes and matrices considered in the current proficiency test. 5.2 Recommendations to the participating laboratories 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. Due to the limited technical information provided by the participants about the details of their analytical procedure, it was not possible to define the detailed root causes of discrepancies. Based on the results of this proficiency test, the analyst could investigate their problems and take necessary remedial actions. Upon a request for assistance on a specific issue, the proficiency test organiser could give technical advice which might help in resolving remaining issues. Therefore, it is recommended, later on, to confirm whether the participating laboratories have gained the capability of analysis of 210Pb through another proficiency test. Laboratory 01 Laboratory 01 reported results for both 137Cs and 210Pb. The uncertainty of 137Cs measurement was around 11%, only for sample 03 was around 22%, which resulted in “warning” score. The laboratory results showed satisfactory repeatability for 137Cs, while it is not the case for 210Pb, up to 20% of difference was observed in measurement of duplicate samples. Root cause of unsatisfactory repeatability of 210Pb should be investigated. In addition, a systematic bias up to 45% is observed in 210Pb results, root cause should be also investigated. The Z-score evaluation results were satisfactory only for 137Cs in all samples. Laboratory 02 Laboratory 02 submitted results both 137Cs and 210Pb. The uncertainty of 137Cs and 210Pb measurement was between 0.8-4.3 %, underestimation of uncertainty in 137Cs for samples 02 and 04 (1%) resulted in “warning” score. According to the reported individual results, the method proves to have a satisfactory repeatability. The bias of 210Pb in sample 03 was significant (25%). In this case root cause should be investigated.

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According to Z-score, the laboratory obtained acceptable scores for all samples except 210Pb in sample 03. Laboratory 03 The laboratory 03 sent results for 137Cs only. The claimed uncertainty of 137Cs was between 3.4-12 %. The laboratory results showed satisfactory performance regarding repeatability and trueness of 137Cs measurements. In Z-score system the laboratory obtained satisfactory scores for all results. Laboratory 04 Laboratory 04 sent results for 137Cs only. The laboratory results showed satisfactory performance regarding repeatability and trueness of 137Cs measurements. In Z-score system the laboratory performed satisfactory for 137Cs in all samples. Laboratory 07 Laboratory 07 sent results for both 137Cs and 210Pb. The claimed uncertainty of 137Cs and 210Pb measurement was between 2.2-6.8 %. A systematic negative bias (up to 34%) was observed in all results of 210Pb which might suggest a calibration problem. In Z-score system the laboratory performed satisfactory for 137Cs in all samples. Laboratory 08 Laboratory 08 submitted results for both 137Cs and 210Pb. The claimed uncertainty of 137Cs measurement was between 4.7-8.2 %, but for sample 03 it was 37% which caused a “Warning” score. If the analyst reported realistic estimation of uncertainty “Acceptable” final score would’ve been assigned. The laboratory demonstrated satisfactory repeatability in 210Pb analysis for all samples, but the results suffered of a negative bias up to 28%. Corrective actions to improve the accuracy of 210Pb should be investigated. In Z-score system the laboratory performed satisfactory for 137Cs for all samples, but 210Pb failed the Z-Score. Laboratory 09 Laboratory 09 submitted results for both 137Cs and 210Pb. The claimed uncertainty of measurements was between 3.7 – 8.3 %. The laboratory demonstrated acceptable performance for 137Cs and 210Pb for all samples, except for 210Pb in sample 02 obtained “Warning” due to underestimated uncertainty (3.7%). Laboratory 09 obtained acceptable Z-Score for all of the results. Laboratory 10 Laboratory 10 submitted results for 137Cs only. The claimed uncertainty of measurements was between 2.1 – 3.0 %. The laboratory demonstrated satisfactory performance for 137Cs for all samples.

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The laboratory obtained acceptable Z-score for all of the results in all samples. Laboratory 11 Laboratory 11 submitted results for both 137Cs and 210Pb. The claimed uncertainty of measurements was between 2 – 11 %, The laboratory demonstrated satisfactory repeatability for both 137Cs and 210Pb in all samples. 210Pb result in sample 03 was satisfactory, but in the rest of the samples results biased up to 43%, corrective actions to improve the accuracy of 210Pb should be implemented. Laboratory 11 obtained acceptable Z-score for 137Cs in samples 01, 02, 04 and 05. Laboratory 12 Laboratory 12 submitted results for both 137Cs and 210Pb, for sample 05 only 137Cs result was reported. The laboratory demonstrated satisfactory performance for 137Cs. 137Cs result in sample 03 was rejected due to its high bias (53%). The analyst should also investigate the cause of discrepancy in the results of the duplicate test samples. Laboratory 12 obtained acceptable Z-score for all of the results except for 137Cs in samples 03 and 05. Laboratory 13 Laboratory 13 submitted results for both 137Cs and 210Pb. The laboratory demonstrated satisfactory performance for 137Cs for all samples. The laboratory demonstrated satisfactory repeatability in 210Pb analysis for all samples, but the results had a positive bias up to 180%. Corrective actions should be investigated. Laboratory 13 obtained acceptable Z-score for all of the results of 137Cs in all samples. Laboratory 15 Laboratory 15 submitted results for both for 137Cs and 210Pb. The laboratory demonstrated satisfactory performance 137Cs for all samples. The 210Pb results of all samples suffered from negative bias up to 30%. Corrective actions should be investigated. Laboratory 15 obtained acceptable Z-score for all of the results of 137Cs in all samples. Laboratory 16 Laboratory 16 submitted results for 137Cs only. The laboratory demonstrated satisfactory performance for 137Cs for all samples. Laboratory 16 obtained acceptable Z-score for all of the results of 137Cs in all samples. Laboratory 17 Laboratory 17 submitted results for both 137Cs and 210Pb.

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Page 18 18

The laboratory demonstrated satisfactory performance 137Cs and 210Pb for all samples. Laboratory 17 obtained acceptable Z-score for all of the results in all samples. Laboratory 18 Laboratory 18 submitted results for both 137Cs and 210Pb. The laboratory demonstrated satisfactory performance for 137Cs and 210Pb for all samples, except for 210Pb in sample 03. The laboratory demonstrated satisfactory repeatability in all analysis for all samples. Laboratory 18 obtained acceptable Z-score for all of the results in all samples except for 210Pb in sample 03. 6. Conclusions In the frame of the IAEA CRP DI.50.08 “Assess the effectiveness of soil conservation measures for sustainable watershed management using fallout radionuclides”, a proficiency test was organized and conducted by the Chemistry Unit of the IAEA's Seibersdorf Laboratories (Austria). 90 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. 14 laboratories from the 18 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 for determining the laboratories performance. The analytical data evaluation of this proficiency test indicates that 82% of the laboratories reported “acceptable” results for the 137Cs and 33% for 210Pb. In the case of 137Cs, the analytical results were satisfactory, while the 210Pb analysis indicated that most of participants have not yet established the analytical capability of 210Pb using gamma-spectrometry. In general, the analytical uncertainties associated with the results were appropriate for the analytes and matrices considered in the current proficiency test. 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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Page 19

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, Switzerland. 3. MAKAREWICZ, M., Gamma Analysis report, Chemistry Unit, Agency's Laboratories. 4. ISO/IEC Guide 35:2000, Certification of reference materials-General and statistical

principles, ISO, Geneva, Switzerland. 5. BROOKES, C.J., BETTELEY, I.G., LOXTON, S.M.; Fundamentals of Mathematics and

Statistics, Wiley 1979. 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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Page 20 20

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Page 21

APPENDIX A: Performance evaluation sorted by radionuclide

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Page 22 22

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Page 23

Target value: 20.3Uncertainty: 0.50

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 20.70 2.30 11.1% 1.9% 0.19 0.17 0.39 6.07 Acceptable 11.4% Acceptable Acceptable02 20.62 0.27 1.3% 1.5% 0.15 0.55 0.31 1.47 Acceptable 2.8% Acceptable Acceptable03 20.30 0.80 3.9% 0.0% 0.00 -0.01 0.01 2.43 Acceptable 4.6% Acceptable Acceptable04 20.07 1.14 5.7% -1.2% -0.12 -0.19 0.24 3.21 Acceptable 6.2% Acceptable Acceptable07 18.90 0.51 2.7% -6.9% -0.69 -1.97 1.41 1.84 Acceptable 3.7% Acceptable Acceptable08 20.70 1.70 8.2% 1.9% 0.19 0.22 0.39 4.57 Acceptable 8.6% Acceptable Acceptable09 20.77 1.02 4.9% 2.3% 0.23 0.41 0.46 2.93 Acceptable 5.5% Acceptable Acceptable10 20.22 0.52 2.6% -0.4% -0.04 -0.12 0.09 1.86 Acceptable 3.6% Acceptable Acceptable11 22.69 0.81 3.6% 11.7% 1.17 2.50 2.38 2.46 Acceptable 4.3% Acceptable Acceptable12 16.60 3.10 18.7% -18.3% -1.83 -1.18 3.71 8.10 Acceptable 18.8% Acceptable Acceptable13 21.91 1.25 5.7% 7.9% 0.79 1.19 1.60 3.47 Acceptable 6.2% Acceptable Acceptable15 19.66 0.72 3.7% -3.2% -0.32 -0.74 0.65 2.26 Acceptable 4.4% Acceptable Acceptable16 20.85 1.00 4.8% 2.7% 0.27 0.49 0.54 2.88 Acceptable 5.4% Acceptable Acceptable17 20.95 0.46 2.2% 3.2% 0.32 0.95 0.64 1.75 Acceptable 3.3% Acceptable Acceptable18 19.90 0.80 4.0% -2.0% -0.20 -0.43 0.41 2.43 Acceptable 4.7% Acceptable Acceptable

Table legend:

A1:

A2:

P:

[Bq/kg]

0.93

1.08

1.12

Bias(%) Z-Score U-Score Lab./IAEA1.02

1.02

Data Evaluation of 137Cs in spiked soil, sample code 01

0.971.03

1.021.000.99

1.030.98

1.021.00

0.82

5.0

10.0

15.0

20.0

25.0

30.0

35.0

01 02 03 04 07 08 09 10 11 12 13 15 16 17 18Laboratory Code

137 C

s Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

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Page 24 24

Target value: 289Uncertainty: 7.0

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 195.00 55.00 28.2% -32.5% -3.25 -1.70 94.00 143.04 Acceptable 28.3% Not Acceptable Not Acceptable02 293.13 3.17 1.1% 1.4% 0.14 0.54 4.13 19.83 Acceptable 2.7% Acceptable Acceptable07 229.04 7.82 3.4% -20.7% -2.07 -5.71 59.96 27.08 Not Acceptable 4.2% Acceptable Warning08 212.00 22.40 10.6% -26.6% -2.66 -3.28 77.00 60.55 Not Acceptable 10.8% Acceptable Not Acceptable09 261.50 14.20 5.4% -9.5% -0.95 -1.74 27.50 40.85 Acceptable 5.9% Acceptable Acceptable11 170.64 5.25 3.1% -41.0% -4.10 -13.53 118.36 22.58 Not Acceptable 3.9% Acceptable Not Acceptable12 271.00 10.84 4.0% -6.2% -0.62 -1.39 18.00 33.29 Acceptable 4.7% Acceptable Acceptable13 650.10 37.80 5.8% 124.9% 12.49 9.39 361.10 99.18 Not Acceptable 6.3% Acceptable Not Acceptable15 232.88 6.47 2.8% -19.4% -1.94 -5.89 56.12 24.59 Not Acceptable 3.7% Acceptable Warning17 290.00 16.00 5.5% 0.3% 0.03 0.06 1.00 45.06 Acceptable 6.0% Acceptable Acceptable18 316.50 17.30 5.5% 9.5% 0.95 1.47 27.50 48.15 Acceptable 6.0% Acceptable Acceptable

Table legend:

A1:

A2:

P:

0.81

0.590.942.25

1.010.790.730.90

1.10

[Bq/kg] Data Evaluation of 210Pb in spiked soil, sample code 01

Bias(%) Z-Score U-Score Lab/IAEA

1.00

0.67

140.0

180.0

220.0

260.0

300.0

340.0

380.0

420.0

01 02 07 08 09 11 12 13 15 17 18Laboratory Code

210 P

b Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

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Page 25

Target value: 38.4Uncertainty: 0.83

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 38.50 4.30 11.2% 0.3% 0.03 0.02 0.10 11.30 Acceptable 11.4% Acceptable Acceptable02 41.59 0.42 1.0% 8.3% 0.83 3.43 3.19 2.40 Not Acceptable 2.4% Acceptable Warning03 38.00 1.30 3.4% -1.0% -0.10 -0.26 0.40 3.98 Acceptable 4.0% Acceptable Acceptable04 39.07 2.18 5.6% 1.7% 0.17 0.29 0.67 6.02 Acceptable 6.0% Acceptable Acceptable07 35.58 0.80 2.2% -7.3% -0.73 -2.45 2.82 2.97 Acceptable 3.1% Acceptable Acceptable08 40.40 1.90 4.7% 5.2% 0.52 0.96 2.00 5.35 Acceptable 5.2% Acceptable Acceptable09 39.32 1.74 4.4% 2.4% 0.24 0.48 0.92 4.97 Acceptable 4.9% Acceptable Acceptable10 38.44 0.94 2.4% 0.1% 0.01 0.03 0.04 3.24 Acceptable 3.3% Acceptable Acceptable11 41.49 0.92 2.2% 8.0% 0.80 2.49 3.09 3.20 Acceptable 3.1% Acceptable Acceptable12 33.50 2.20 6.6% -12.8% -1.28 -2.08 4.90 6.07 Acceptable 6.9% Acceptable Acceptable13 45.92 2.42 5.3% 19.6% 1.96 2.94 7.52 6.60 Not Acceptable 5.7% Acceptable Warning15 39.51 0.89 2.3% 2.9% 0.29 0.91 1.11 3.14 Acceptable 3.1% Acceptable Acceptable16 40.00 0.80 2.0% 4.2% 0.42 1.39 1.60 2.97 Acceptable 2.9% Acceptable Acceptable17 43.13 0.79 1.8% 12.3% 1.23 4.13 4.73 2.96 Not Acceptable 2.8% Acceptable Warning18 40.50 1.30 3.2% 5.5% 0.55 1.36 2.10 3.98 Acceptable 3.9% Acceptable Acceptable

Table legend:

A1:

A2:

P:

1.121.05

1.021.00

0.87

1.05

Data Evaluation of 137Cs in spiked soil, sample code 02

1.031.04

1.080.991.02

[Bq/kg]

0.93

1.20

1.08

Bias(%) Z-Score U-Score Lab./IAEA1.00

25.0

30.0

35.0

40.0

45.0

50.0

55.0

01 02 03 04 07 08 09 10 11 12 13 15 16 17 18Laboratory Code

137 C

s Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

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Page 26 26

Target value: 530Uncertainty: 11.3

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 340.00 76.00 22.4% -35.8% -3.58 -2.47 0.64 190.00 198.24 Acceptable 22.5% Not Acceptable Not Acceptable02 532.87 4.57 0.9% 0.5% 0.05 0.24 1.01 2.87 31.45 Acceptable 2.3% Acceptable Acceptable07 379.56 12.02 3.2% -28.4% -2.84 -9.12 0.72 150.44 42.56 Not Acceptable 3.8% Acceptable Not Acceptable08 415.30 27.40 6.6% -21.6% -2.16 -3.87 0.78 114.70 76.47 Not Acceptable 6.9% Acceptable Not Acceptable09 475.80 17.70 3.7% -10.2% -1.02 -2.58 0.90 54.20 54.18 Not Acceptable 4.3% Acceptable Warning11 301.33 7.44 2.5% -43.1% -4.31 -16.90 0.57 228.67 34.91 Not Acceptable 3.3% Acceptable Not Acceptable12 538.00 21.52 4.0% 1.5% 0.15 0.33 1.02 8.00 62.71 Acceptable 4.5% Acceptable Acceptable13 1257.20 66.30 5.3% 137.2% 13.72 10.81 2.37 727.20 173.52 Not Acceptable 5.7% Acceptable Not Acceptable15 370.62 6.29 1.7% -30.1% -3.01 -12.32 0.70 159.38 33.37 Not Acceptable 2.7% Acceptable Not Acceptable17 543.00 24.00 4.4% 2.5% 0.25 0.49 1.02 13.00 68.44 Acceptable 4.9% Acceptable Acceptable18 602.10 31.40 5.2% 13.6% 1.36 2.16 72.10 86.10 Acceptable 5.6% Acceptable Acceptable

Table legend1.14

[Bq/kg] Data Evaluation of 210Pb in spiked soil, sample code 02

Bias(%) Z-Score U-Score Laboratory/IAEA

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

290.0

350.0

410.0

470.0

530.0

590.0

650.0

710.0

0 1 0 2 0 7 0 8 0 9 1 1 1 2 1 3 1 5 1 7 1 8

Laboratory Code

210 P

b Acti

vity [

Bq/K

g]

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Page 27

Target value: 2.62Uncertainty: 0.20

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 2.30 0.50 21.7% -12.2% -1.22 -0.59 0.32 1.39 Acceptable 23.0% Not Acceptable Warning02 2.79 0.12 4.3% 6.5% 0.65 0.73 0.17 0.60 Acceptable 8.8% Acceptable Acceptable03 2.50 0.30 12.0% -4.6% -0.46 -0.33 0.12 0.93 Acceptable 14.2% Acceptable Acceptable04 2.44 0.21 8.6% -6.9% -0.69 -0.62 0.18 0.75 Acceptable 11.5% Acceptable Acceptable07 2.37 0.16 6.8% -9.5% -0.95 -0.98 0.25 0.66 Acceptable 10.2% Acceptable Acceptable08 2.70 1.00 37.0% 3.1% 0.31 0.08 0.08 2.63 Acceptable 37.8% Not Acceptable Warning09 2.42 0.20 8.3% -7.6% -0.76 -0.71 0.20 0.73 Acceptable 11.3% Acceptable Acceptable10 2.98 0.09 3.0% 13.7% 1.37 1.64 0.36 0.57 Acceptable 8.2% Acceptable Acceptable11 4.49 0.49 10.9% 71.4% 7.14 3.53 1.87 1.37 Not Acceptable 13.3% Acceptable Not Acceptable12 4.00 1.60 40.0% 52.7% 5.27 0.86 1.38 4.16 Acceptable 40.7% Not Acceptable Not Acceptable13 3.04 0.39 12.8% 16.0% 1.60 0.96 0.42 1.13 Acceptable 14.9% Acceptable Acceptable15 2.84 0.49 17.3% 8.4% 0.84 0.42 0.22 1.37 Acceptable 18.9% Acceptable Acceptable16 3.17 0.22 6.9% 21.0% 2.10 1.85 0.55 0.77 Acceptable 10.3% Acceptable Acceptable17 2.83 0.23 8.1% 8.0% 0.80 0.69 0.21 0.79 Acceptable 11.2% Acceptable Acceptable18 2.50 0.30 12.0% -4.6% -0.46 -0.33 0.12 0.93 Acceptable 14.2% Acceptable Acceptable

Table legend:

A1:

A2:

P:

[Bq/kg]

0.90

1.16

1.71

Bias(%) Z-Score U-Score Lab./IAEA0.88

1.03

Data Evaluation of 137Cs in spiked soil, sample code 03

1.081.21

1.060.950.93

1.080.95

0.921.14

1.53

0.6

1.1

1.6

2.1

2.6

3.1

3.6

4.1

4.6

01 02 03 04 07 08 09 10 11 12 13 15 16 17 18Laboratory Code

137 C

s Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

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Page 28 28

Target value: 48Uncertainty: 1.5

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 44.00 20.00 45.5% -8.3% -0.83 -0.20 0.92 4.00 51.74 Acceptable 45.6% Not Acceptable Warning02 59.95 1.69 2.8% 24.9% 2.49 5.29 1.25 11.95 5.83 Not Acceptable 4.2% Acceptable Warning07 45.46 2.52 5.5% -5.3% -0.53 -0.87 0.95 2.54 7.57 Acceptable 6.4% Acceptable Acceptable08 59.10 22.60 38.2% 23.1% 2.31 0.49 1.23 11.10 58.44 Acceptable 38.4% Not Acceptable Warning09 49.92 3.51 7.0% 4.0% 0.40 0.50 1.04 1.92 9.85 Acceptable 7.7% Acceptable Acceptable11 46.22 4.82 10.4% -3.7% -0.37 -0.35 0.96 1.78 13.02 Acceptable 10.9% Acceptable Acceptable12 40.00 1.60 4.0% -16.7% -1.67 -3.65 0.83 8.00 5.66 Not Acceptable 5.1% Acceptable Warning13 135.20 13.80 10.2% 181.7% 18.17 6.28 2.82 87.20 35.81 Not Acceptable 10.7% Acceptable Not Acceptable15 37.08 3.96 10.7% -22.8% -2.28 -2.58 0.77 10.92 10.93 Acceptable 11.1% Acceptable Acceptable17 48.00 9.00 18.8% 0.0% 0.00 0.00 1.00 0.00 23.54 Acceptable 19.0% Acceptable Acceptable18 64.10 4.00 6.2% 33.5% 3.35 3.77 16.10 11.02 Not Acceptable 7.0% Acceptable Not Acceptable

Table legend:

A1:

A2:

P:

1.34

[Bq/kg] Data Evaluation of 210Pb in spiked soil, sample code 03

Bias(%) Z-Score U-Score Laboratory/IAEA

28.0

38.0

48.0

58.0

68.0

01 02 07 08 09 11 12 13 15 17 18Laboratory Code

238 U

Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

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Page 29

Target value: 38.4Uncertainty: 0.83

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 40.80 4.60 11.3% 6.2% 0.62 0.51 2.38 12.06 Acceptable 11.5% Acceptable Acceptable02 41.76 0.36 0.9% 8.7% 0.87 3.70 3.34 2.33 Not Acceptable 2.3% Acceptable Warning03 39.10 1.40 3.6% 1.8% 0.18 0.42 0.68 4.19 Acceptable 4.2% Acceptable Acceptable04 39.73 2.21 5.6% 3.4% 0.34 0.55 1.31 6.09 Acceptable 6.0% Acceptable Acceptable07 33.83 0.78 2.3% -12.0% -1.20 -4.04 4.59 2.93 Not Acceptable 3.2% Acceptable Warning08 40.50 1.90 4.7% 5.4% 0.54 1.00 2.08 5.35 Acceptable 5.2% Acceptable Acceptable09 42.60 1.88 4.4% 10.9% 1.09 2.03 4.18 5.30 Acceptable 4.9% Acceptable Acceptable10 38.14 0.93 2.4% -0.7% -0.07 -0.23 0.28 3.21 Acceptable 3.3% Acceptable Acceptable11 40.19 0.78 1.9% 4.6% 0.46 1.55 1.77 2.93 Acceptable 2.9% Acceptable Acceptable12 36.90 4.10 11.1% -4.0% -0.40 -0.36 1.52 10.79 Acceptable 11.3% Acceptable Acceptable13 45.10 2.37 5.3% 17.4% 1.74 2.66 6.68 6.48 Not Acceptable 5.7% Acceptable Warning15 38.32 0.85 2.2% -0.3% -0.03 -0.09 0.10 3.06 Acceptable 3.1% Acceptable Acceptable16 38.56 0.80 2.1% 0.4% 0.04 0.12 0.14 2.97 Acceptable 3.0% Acceptable Acceptable17 43.40 0.79 1.8% 12.9% 1.29 4.35 4.98 2.95 Not Acceptable 2.8% Acceptable Warning18 39.90 1.20 3.0% 3.8% 0.38 1.01 1.48 3.76 Acceptable 3.7% Acceptable Acceptable

Table legend:

A1:

A2:

P:

[Bq/kg]

0.88

1.17

1.05

Bias(%) Z-Score U-Score Lab./IAEA1.06

1.05

Data Evaluation of 137Cs in spiked soil, sample code 04

1.001.00

1.091.021.03

1.131.04

1.110.99

0.96

23.0

28.0

33.0

38.0

43.0

48.0

53.0

01 02 03 04 07 08 09 10 11 12 13 15 16 17 18Laboratory Code

137 C

s Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

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Page 30 30

Target value: 530Uncertainty: 11.3

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 290.00 82.00 28.3% -45.3% -4.53 -2.90 0.55 240.00 213.56 Not Acceptable 28.4% Not Acceptable Not Acceptable02 540.31 4.27 0.8% 1.9% 0.19 0.85 1.02 10.31 31.17 Acceptable 2.3% Acceptable Acceptable07 348.12 11.02 3.2% -34.3% -3.43 -11.52 0.66 181.88 40.72 Not Acceptable 3.8% Acceptable Not Acceptable08 381.00 24.70 6.5% -28.1% -2.81 -5.49 0.72 149.00 70.08 Not Acceptable 6.8% Acceptable Not Acceptable09 484.60 19.20 4.0% -8.6% -0.86 -2.04 0.91 45.40 57.48 Acceptable 4.5% Acceptable Acceptable11 279.91 8.74 3.1% -47.2% -4.72 -17.51 0.53 250.09 36.86 Not Acceptable 3.8% Acceptable Not Acceptable12 467.00 18.68 4.0% -11.9% -1.19 -2.89 0.88 63.00 56.33 Not Acceptable 4.5% Acceptable Warning13 1236.80 65.60 5.3% 133.4% 13.34 10.62 2.33 706.80 171.74 Not Acceptable 5.7% Acceptable Not Acceptable15 372.18 7.94 2.1% -29.8% -2.98 -11.43 0.70 157.82 35.63 Not Acceptable 3.0% Acceptable Not Acceptable17 557.00 25.00 4.5% 5.1% 0.51 0.98 1.05 27.00 70.78 Acceptable 5.0% Acceptable Acceptable18 599.00 32.60 5.4% 13.0% 1.30 2.00 69.00 89.02 Acceptable 5.8% Acceptable Acceptable

Table legend:

A1:

A2:

P:

1.13

[Bq/kg] Data Evaluation of 210Pb in spiked soil, sample code 04

Bias(%) Z-Score U-Score Laboratory/IAEA

290.0

350.0

410.0

470.0

530.0

590.0

650.0

710.0

01 02 07 08 09 11 12 13 15 17 18Laboratory Code

210 P

b Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

Page 32: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 31

Target value: 20.3Uncertainty: 0.50

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 20.30 2.30 11.3% 0.0% 0.00 0.00 0.00 6.07 Acceptable 11.6% Acceptable Acceptable02 21.18 0.23 1.1% 4.3% 0.43 1.60 0.88 1.42 Acceptable 2.7% Acceptable Acceptable03 19.80 0.80 4.0% -2.5% -0.25 -0.53 0.50 2.43 Acceptable 4.7% Acceptable Acceptable04 20.46 1.14 5.6% 0.8% 0.08 0.13 0.16 3.21 Acceptable 6.1% Acceptable Acceptable07 19.32 0.49 2.5% -4.8% -0.48 -1.40 0.98 1.81 Acceptable 3.5% Acceptable Acceptable08 20.20 1.60 7.9% -0.5% -0.05 -0.06 0.10 4.32 Acceptable 8.3% Acceptable Acceptable09 21.95 1.61 7.3% 8.1% 0.81 0.98 1.65 4.35 Acceptable 7.7% Acceptable Acceptable10 19.99 0.42 2.1% -1.5% -0.15 -0.47 0.31 1.68 Acceptable 3.2% Acceptable Acceptable11 21.07 0.62 2.9% 3.8% 0.38 0.97 0.77 2.05 Acceptable 3.8% Acceptable Acceptable12 12.70 3.10 24.4% -37.4% -3.74 -2.42 7.60 8.10 Acceptable 24.5% Not Acceptable Not Acceptable13 22.54 1.25 5.5% 11.0% 1.10 1.66 2.24 3.47 Acceptable 6.1% Acceptable Acceptable15 18.46 0.42 2.3% -9.1% -0.91 -2.82 1.84 1.68 Not Acceptable 3.4% Acceptable Warning16 20.86 1.00 4.8% 2.8% 0.28 0.50 0.56 2.88 Acceptable 5.4% Acceptable Acceptable17 21.01 0.62 3.0% 3.5% 0.35 0.89 0.71 2.05 Acceptable 3.8% Acceptable Acceptable18 20.30 0.80 3.9% 0.0% 0.00 0.00 0.00 2.43 Acceptable 4.6% Acceptable Acceptable

Table legend:

A1:

A2:

P:

1.031.00

1.080.98

0.63

1.00

Data Evaluation of 137Cs in spiked soil, sample code 05

0.911.03

1.040.981.01

[Bq/kg]

0.95

1.11

1.04

Bias(%) Z-Score U-Score Lab./IAEA1.00

0.0

5.0

10.0

15.0

20.0

25.0

30.0

01 02 03 04 07 08 09 10 11 12 13 15 16 17 18Laboratory Code

137 C

s Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

Page 33: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 32 32

Target value: 289.0Uncertainty: 6.98

Laboratories Results Acceptance criteria FinalLab. Code Value Unc. Trueness Precision Score

[Bq/kg] [Bq/kg] % A1 A2 Score P Score01 160.00 58.00 36.3% -44.6% -4.46 -2.21 129.00 150.72 Acceptable 36.3% Not Acceptable Not Acceptable02 300.44 2.92 1.0% 4.0% 0.40 1.51 11.44 19.53 Acceptable 2.6% Acceptable Acceptable07 213.26 7.05 3.3% -26.2% -2.62 -7.63 75.74 25.60 Not Acceptable 4.1% Acceptable Not Acceptable08 206.70 24.00 11.6% -28.5% -2.85 -3.29 82.30 64.49 Not Acceptable 11.9% Acceptable Not Acceptable09 272.30 12.70 4.7% -5.8% -0.58 -1.15 16.70 37.39 Acceptable 5.3% Acceptable Acceptable11 177.00 6.85 3.9% -38.8% -3.88 -11.45 112.00 25.24 Not Acceptable 4.6% Acceptable Not Acceptable13 655.90 36.40 5.5% 127.0% 12.70 9.90 366.90 95.62 Not Acceptable 6.1% Acceptable Not Acceptable15 199.53 5.26 2.6% -31.0% -3.10 -10.23 89.47 22.55 Not Acceptable 3.6% Acceptable Not Acceptable17 250.00 16.00 6.4% -13.5% -1.35 -2.23 39.00 45.04 Acceptable 6.8% Acceptable Acceptable18 310.40 18.10 5.8% 7.4% 0.74 1.10 21.40 50.05 Acceptable 6.3% Acceptable Acceptable

Table legend:

A1:

A2:

P:

0.871.07

2.270.69

0.61

0.740.720.94

[Bq/kg]

0.551.04

Data Evaluation of 210Pb in spiked soil, sample code 05

Bias(%) Z-Score U-Score Lab./IAEA

150.0

175.0

200.0

225.0

250.0

275.0

300.0

325.0

350.0

01 02 07 08 09 11 13 15 17 18Laboratory Code

210 P

b Acti

vity [

Bq/K

g]

LaboratoryIAEA ValueValue −

2258.2 LaboratoryIAEA UncUnc +×

%1002

.

2

XValueUnc

ValueUnc

Lab

Lab

IAEA

IAEA

+

Page 34: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 33

APPENDIX B: Performance evaluation sorted by laboratory code

Page 35: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 34 34

Page 36: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 35

Analytical Performance Evaluation of Laboratory 01137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.7 2.3 11.1% 2% 0.19 0.17 0.39 6.07 Acceptable 11.4% Acceptable Acceptable210Pb 01 289.0 7.0 195.0 55.0 28.2% -33% -3.25 -1.70 94.00 143.04 Acceptable 28.3% Not Acceptable Not Acceptable137Cs 02 38.4 0.8 38.5 4.3 11.2% 0% 0.03 0.02 0.10 11.30 Acceptable 11.4% Acceptable Acceptable210Pb 02 530.0 11.3 340.0 76.0 22.4% -36% -3.58 -2.47 190.00 198.24 Acceptable 22.5% Not Acceptable Not Acceptable137Cs 03 2.6 0.2 2.3 0.5 21.7% -12% -1.22 -0.59 0.32 1.39 Acceptable 23.0% Not Acceptable Warning210Pb 03 48.0 1.5 44.0 20.0 45.5% -8% -0.83 -0.20 4.00 51.74 Acceptable 45.6% Not Acceptable Warning137Cs 04 38.4 0.8 40.8 4.6 11.3% 6% 0.62 0.51 2.38 12.06 Acceptable 11.5% Acceptable Acceptable210Pb 04 530.0 11.3 290.0 82.0 28.3% -45% -4.53 -2.90 240.00 213.56 Not Acceptable 28.4% Not Acceptable Not Acceptable137Cs 05 20.3 0.5 20.3 2.3 11.3% 0% 0.00 0.00 0.00 6.07 Acceptable 11.6% Acceptable Acceptable210Pb 05 289.0 7.0 160.0 58.0 36.3% -45% -4.46 -2.21 129.00 150.72 Acceptable 36.3% Not Acceptable Not Acceptable0.55

0.880.921.060.55

0.671.000.64

1.00

Samplecode

LaboratoryLab./IAEA

1.02

Page 37: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 36 36

Analytical Performance Evaluation of Laboratory 02137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.62 0.27 1.3% 2% 0.15 0.55 0.31 1.47 Acceptable 2.8% Acceptable Acceptable210Pb 01 289.0 7.0 293.13 3.17 1.1% 1% 0.14 0.54 4.13 19.83 Acceptable 2.7% Acceptable Acceptable137Cs 02 38.4 0.8 41.59 0.42 1.0% 8% 0.83 3.43 3.19 2.40 Not Acceptable 2.4% Acceptable Warning210Pb 02 530.0 11.3 532.87 4.57 0.9% 1% 0.05 0.24 2.87 31.45 Acceptable 2.3% Acceptable Acceptable137Cs 03 2.6 0.2 2.79 0.12 4.3% 6% 0.65 0.73 0.17 0.60 Acceptable 8.8% Acceptable Acceptable210Pb 03 48.0 1.5 59.95 1.69 2.8% 25% 2.49 5.29 11.95 5.83 Not Acceptable 4.2% Acceptable Not Acceptable137Cs 04 38.4 0.8 41.76 0.36 0.9% 9% 0.87 3.70 3.34 2.33 Not Acceptable 2.3% Acceptable Warning210Pb 04 530.0 11.3 540.31 4.27 0.8% 2% 0.19 0.85 10.31 31.17 Acceptable 2.3% Acceptable Acceptable137Cs 05 20.3 0.5 21.18 0.23 1.1% 4% 0.43 1.60 0.88 1.42 Acceptable 2.7% Acceptable Acceptable210Pb 05 289.0 7.0 300.44 2.92 1.0% 4% 0.40 1.51 11.44 19.53 Acceptable 2.6% Acceptable Acceptable1.04

1.061.251.091.02

1.011.081.01

1.04

Samplecode

LaboratoryLab./IAEA

1.02

Page 38: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 37

Analytical Performance Evaluation of Laboratory 03137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.3 0.8 3.9% 0% 0.00 -0.01 0.01 2.43 Acceptable 4.6% Acceptable Acceptable137Cs 02 38.4 0.8 38.0 1.3 3.4% -1% -0.10 -0.26 0.40 3.98 Acceptable 4.0% Acceptable Acceptable137Cs 03 2.6 0.2 2.5 0.3 12.0% -5% -0.46 -0.33 0.12 0.93 Acceptable 14.2% Acceptable Acceptable137Cs 04 38.4 0.8 39.1 1.4 3.6% 2% 0.18 0.42 0.68 4.19 Acceptable 4.2% Acceptable Acceptable137Cs 05 20.3 0.5 19.8 0.8 4.0% -2% -0.25 -0.53 0.50 2.43 Acceptable 4.7% Acceptable Acceptable

0.990.951.020.98

Samplecode

LaboratoryLab./IAEA

1.00

Analytical Performance Evaluation of Laboratory 04137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.1 1.1 5.7% -1% -0.12 -0.19 0.24 3.21 Acceptable 6.2% Acceptable Acceptable137Cs 02 38.4 0.8 39.1 2.2 5.6% 2% 0.17 0.29 0.67 6.02 Acceptable 6.0% Acceptable Acceptable137Cs 03 2.6 0.2 2.4 0.2 8.6% -7% -0.69 -0.62 0.18 0.75 Acceptable 11.5% Acceptable Acceptable137Cs 04 38.4 0.8 39.7 2.2 5.6% 3% 0.34 0.55 1.31 6.09 Acceptable 6.0% Acceptable Acceptable137Cs 05 20.3 0.5 20.5 1.1 5.6% 1% 0.08 0.13 0.16 3.21 Acceptable 6.1% Acceptable Acceptable

1.020.931.031.01

Samplecode

LaboratoryLab./IAEA

0.99

Page 39: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 38 38

Analytical Performance Evaluation of Laboratory 07137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 18.9 0.5 2.7% -7% -0.69 -1.97 1.41 1.84 Acceptable 3.7% Acceptable Acceptable210Pb 01 289.0 7.0 229.0 7.8 3.4% -21% -2.07 -5.71 59.96 27.08 Not Acceptable 4.2% Acceptable Not Acceptable137Cs 02 38.4 0.8 35.6 0.8 2.2% -7% -0.73 -2.45 2.82 2.97 Acceptable 3.1% Acceptable Acceptable210Pb 02 530.0 11.3 379.6 12.0 3.2% -28% -2.84 -9.12 150.44 42.56 Not Acceptable 3.8% Acceptable Not Acceptable137Cs 03 2.6 0.2 2.4 0.2 6.8% -10% -0.95 -0.98 0.25 0.66 Acceptable 10.2% Acceptable Acceptable210Pb 03 48.0 1.5 45.5 2.5 5.5% -5% -0.53 -0.87 2.54 7.57 Acceptable 6.4% Acceptable Acceptable137Cs 04 38.4 0.8 33.8 0.8 2.3% -12% -1.20 -4.04 4.59 2.93 Not Acceptable 3.2% Acceptable Warning210Pb 04 530.0 11.3 348.1 11.0 3.2% -34% -3.43 -11.52 181.88 40.72 Not Acceptable 3.8% Acceptable Not Acceptable137Cs 05 20.3 0.5 19.3 0.5 2.5% -5% -0.48 -1.40 0.98 1.81 Acceptable 3.5% Acceptable Acceptable210Pb 05 289.0 7.0 213.3 7.1 3.3% -26% -2.62 -7.63 75.74 25.60 Not Acceptable 4.1% Acceptable Not Acceptable0.74

0.950.880.660.95

0.790.930.720.90

Samplecode

LaboratoryLab./IAEA

0.93

Page 40: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 39

Analytical Performance Evaluation of Laboratory 08137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.7 1.7 8.2% 2% 0.19 0.22 0.39 4.57 Acceptable 8.6% Acceptable Acceptable210Pb 01 289.0 7.0 212.0 22.4 10.6% -27% -2.66 -3.28 77.00 60.55 Not Acceptable 10.8% Acceptable Not Acceptable137Cs 02 38.4 0.8 40.4 1.9 4.7% 5% 0.52 0.96 2.00 5.35 Acceptable 5.2% Acceptable Acceptable210Pb 02 530.0 11.3 415.3 27.4 6.6% -22% -2.16 -3.87 114.70 76.47 Not Acceptable 6.9% Acceptable Not Acceptable137Cs 03 2.6 0.2 2.7 1.0 37.0% 3% 0.31 0.08 0.08 2.63 Acceptable 37.8% Not Acceptable Warning210Pb 03 48.0 1.5 59.1 22.6 38.2% 23% 2.31 0.49 11.10 58.44 Acceptable 38.4% Not Acceptable Not Acceptable137Cs 04 38.4 0.8 40.5 1.9 4.7% 5% 0.54 1.00 2.08 5.35 Acceptable 5.2% Acceptable Acceptable210Pb 04 530.0 11.3 381.0 24.7 6.5% -28% -2.81 -5.49 149.00 70.08 Not Acceptable 6.8% Acceptable Not Acceptable137Cs 05 20.3 0.5 20.2 1.6 7.9% 0% -0.05 -0.06 0.10 4.32 Acceptable 8.3% Acceptable Acceptable210Pb 05 289.0 7.0 206.7 24.0 11.6% -28% -2.85 -3.29 82.30 64.49 Not Acceptable 11.9% Acceptable Not Acceptable0.72

1.231.050.721.00

0.731.050.781.03

Samplecode

LaboratoryLab./IAEA

1.02

Page 41: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 40 40

Analytical Performance Evaluation of Laboratory 09137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.77 1.02 4.9% 2% 0.23 0.41 0.46 2.93 Acceptable 5.5% Acceptable Acceptable210Pb 01 289.0 7.0 261.5 14.20 5.4% -10% -0.95 -1.74 27.50 40.85 Acceptable 5.9% Acceptable Acceptable137Cs 02 38.4 0.8 39.32 1.74 4.4% 2% 0.24 0.48 0.92 4.97 Acceptable 4.9% Acceptable Acceptable210Pb 02 530.0 11.3 475.8 17.70 3.7% -10% -1.02 -2.58 54.20 54.18 Not Acceptable 4.3% Acceptable Warning137Cs 03 2.6 0.2 2.42 0.20 8.3% -8% -0.76 -0.71 0.20 0.73 Acceptable 11.3% Acceptable Acceptable210Pb 03 48.0 1.5 49.92 3.51 7.0% 4% 0.40 0.50 1.92 9.85 Acceptable 7.7% Acceptable Acceptable137Cs 04 38.4 0.8 42.60 1.88 4.4% 11% 1.09 2.03 4.18 5.30 Acceptable 4.9% Acceptable Acceptable210Pb 04 530.0 11.3 484.6 19.20 4.0% -9% -0.86 -2.04 45.40 57.48 Acceptable 4.5% Acceptable Acceptable137Cs 05 20.3 0.5 21.95 1.61 7.3% 8% 0.81 0.98 1.65 4.35 Acceptable 7.7% Acceptable Acceptable210Pb 05 289.0 7.0 272.3 12.70 4.7% -6% -0.58 -1.15 16.70 37.39 Acceptable 5.3% Acceptable Acceptable0.94

1.041.110.911.08

0.901.020.900.92

Samplecode

LaboratoryLab./IAEA

1.02

Page 42: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 41

Analytical Performance Evaluation of Laboratory 10137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.22 0.52 2.6% 0% -0.04 -0.12 0.09 1.86 Acceptable 3.6% Acceptable Acceptable137Cs 02 38.4 0.8 38.44 0.94 2.4% 0% 0.01 0.03 0.04 3.24 Acceptable 3.3% Acceptable Acceptable137Cs 03 2.6 0.2 2.98 0.09 3.0% 14% 1.37 1.64 0.36 0.57 Acceptable 8.2% Acceptable Acceptable137Cs 04 38.4 0.8 38.14 0.93 2.4% -1% -0.07 -0.23 0.28 3.21 Acceptable 3.3% Acceptable Acceptable137Cs 05 20.3 0.5 19.99 0.42 2.1% -2% -0.15 -0.47 0.31 1.68 Acceptable 3.2% Acceptable Acceptable

1.140.99

1.00

0.98

Samplecode

LaboratoryLab./IAEA

1.00

Page 43: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 42 42

Analytical Performance Evaluation of Laboratory 11137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 22.7 0.8 3.6% 12% 1.17 2.50 2.38 2.46 Acceptable 4.3% Acceptable Acceptable210Pb 01 289.0 7.0 170.6 5.3 3.1% -41% -4.10 -13.53 118.36 22.58 Not Acceptable 3.9% Acceptable Not Acceptable137Cs 02 38.4 0.8 41.5 0.9 2.2% 8% 0.80 2.49 3.09 3.20 Acceptable 3.1% Acceptable Acceptable210Pb 02 530.0 11.3 301.3 0.0 0.0% -43% -4.31 -20.24 228.67 29.15 Not Acceptable 2.1% Acceptable Not Acceptable137Cs 03 2.6 0.2 4.5 0.5 10.9% 71% 7.14 3.53 1.87 1.37 Not Acceptable 13.3% Acceptable Not Acceptable210Pb 03 48.0 1.5 46.2 4.8 10.4% -4% -0.37 -0.35 1.78 13.02 Acceptable 10.9% Acceptable Acceptable137Cs 04 38.4 0.8 40.2 0.8 1.9% 5% 0.46 1.55 1.77 2.93 Acceptable 2.9% Acceptable Acceptable210Pb 04 530.0 11.3 279.9 8.7 3.1% -47% -4.72 -17.51 250.09 36.86 Not Acceptable 3.8% Acceptable Not Acceptable137Cs 05 20.3 0.5 21.1 0.6 2.9% 4% 0.38 0.97 0.77 2.05 Acceptable 3.8% Acceptable Acceptable210Pb 05 289.0 7.0 177.0 6.9 3.9% -39% -3.88 -11.45 112.00 25.24 Not Acceptable 4.6% Acceptable Not Acceptable0.61

1.710.961.050.53

0.591.080.57

1.04

Samplecode

LaboratoryLab./IAEA

1.12

Page 44: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 43

Analytical Performance Evaluation of Laboratory 12137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 16.6 3.1 18.7% -18% -1.83 -1.18 3.71 8.10 Acceptable 18.8% Acceptable Acceptable210Pb 01 289.0 7.0 271.0 10.8 4.0% -6% -0.62 -1.39 18.00 33.29 Acceptable 4.7% Acceptable Acceptable137Cs 02 38.4 0.8 33.5 2.2 6.6% -13% -1.28 -2.08 4.90 6.07 Acceptable 6.9% Acceptable Acceptable210Pb 02 530.0 11.3 538.0 21.5 4.0% 2% 0.15 0.33 8.00 62.71 Acceptable 4.5% Acceptable Acceptable137Cs 03 2.6 0.2 4.0 1.6 40.0% 53% 5.27 0.86 1.38 4.16 Acceptable 40.7% Not Acceptable Not Acceptable210Pb 03 48.0 1.5 40.0 1.6 4.0% -17% -1.67 -3.65 8.00 5.66 Not Acceptable 5.1% Acceptable Warning137Cs 04 38.4 0.8 36.9 4.1 11.1% -4% -0.40 -0.36 1.52 10.79 Acceptable 11.3% Acceptable Acceptable210Pb 04 530.0 11.3 467.0 18.7 4.0% -12% -1.19 -2.89 63.00 56.33 Not Acceptable 4.5% Acceptable Warning137Cs 05 20.3 0.5 12.7 3.1 24.4% -37% -3.74 -2.42 7.60 8.10 Acceptable 24.5% Not Acceptable Not Acceptable210Pb 05 289.0 7.0 Not reported

1.530.830.960.88

0.940.871.02

0.63

Samplecode

LaboratoryLab./IAEA

0.82

Page 45: Report Pb Cs final · IAEA / AL / 166 Report IAEA-CU-2006-02 Proficiency Test on the Determination of 137 Cs and 210 Pb in spiked soil CRP DI.50.08 "Assess the effectiveness of soil

Page 44 44

Analytical Performance Evaluation of Laboratory 13137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 21.91 1.25 5.7% 8% 0.79 1.19 1.60 3.47 Acceptable 6.2% Acceptable Acceptable210Pb 01 289.0 7.0 650.1 37.8 5.8% 125% 12.49 9.39 361.10 99.18 Not Acceptable 6.3% Acceptable Not Acceptable137Cs 02 38.4 0.8 45.92 2.42 5.3% 20% 1.96 2.94 7.52 6.60 Not Acceptable 5.7% Acceptable Warning210Pb 02 530.0 11.3 1257.2 66.3 5.3% 137% 13.72 10.81 727.20 173.52 Not Acceptable 5.7% Acceptable Not Acceptable137Cs 03 2.6 0.2 3.04 0.39 12.8% 16% 1.60 0.96 0.42 1.13 Acceptable 14.9% Acceptable Acceptable210Pb 03 48.0 1.5 135.2 13.8 10.2% 182% 18.17 6.28 87.20 35.81 Not Acceptable 10.7% Acceptable Not Acceptable137Cs 04 38.4 0.8 45.10 2.37 5.3% 17% 1.74 2.66 6.68 6.48 Not Acceptable 5.7% Acceptable Warning210Pb 04 530.0 11.3 1236.8 65.6 5.3% 133% 13.34 10.62 706.80 171.74 Not Acceptable 5.7% Acceptable Not Acceptable137Cs 05 20.3 0.5 22.54 1.25 5.5% 11% 1.10 1.66 2.24 3.47 Acceptable 6.1% Acceptable Acceptable210Pb 05 289.0 7.0 655.9 36.4 5.5% 127% 12.70 9.90 366.90 95.62 Not Acceptable 6.1% Acceptable Not Acceptable2.27

1.162.821.172.33

2.251.202.37

1.11

Samplecode

LaboratoryLab./IAEA

1.08

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Page 45

Analytical Performance Evaluation of Laboratory 15137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 19.66 0.72 3.7% -3% -0.32 -0.74 0.65 2.26 Acceptable 4.4% Acceptable Acceptable210Pb 01 289.0 7.0 232.88 6.47 2.8% -19% -1.94 -5.89 56.12 24.59 Not Acceptable 3.7% Acceptable Warning137Cs 02 38.4 0.8 39.51 0.89 2.3% 3% 0.29 0.91 1.11 3.14 Acceptable 3.1% Acceptable Acceptable210Pb 02 530.0 11.3 370.62 6.29 1.7% -30% -3.01 -12.32 159.38 33.37 Not Acceptable 2.7% Acceptable Not Acceptable137Cs 03 2.6 0.2 2.84 0.49 17.3% 8% 0.84 0.42 0.22 1.37 Acceptable 18.9% Acceptable Acceptable210Pb 03 48.0 1.5 37.08 3.96 10.7% -23% -2.28 -2.58 10.92 10.93 Acceptable 11.1% Acceptable Acceptable137Cs 04 38.4 0.8 38.32 0.85 2.2% 0% -0.03 -0.09 0.10 3.06 Acceptable 3.1% Acceptable Acceptable210Pb 04 530.0 11.3 372.18 7.94 2.1% -30% -2.98 -11.43 157.82 35.63 Not Acceptable 3.0% Acceptable Not Acceptable137Cs 05 20.3 0.5 18.46 0.42 2.3% -9% -0.91 -2.82 1.84 1.68 Not Acceptable 3.4% Acceptable Warning210Pb 05 289.0 7.0 199.53 5.26 2.6% -31% -3.10 -10.23 89.47 22.55 Not Acceptable 3.6% Acceptable Not Acceptable0.69

0.771.000.700.91

0.811.030.701.08

Samplecode

LaboratoryLab./IAEA

0.97

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Page 46 46

Analytical Performance Evaluation of Laboratory 16137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.9 1.0 4.8% 3% 0.27 0.49 0.54 2.88 Acceptable 5.4% Acceptable Acceptable137Cs 02 38.4 0.8 40.0 0.8 2.0% 4% 0.42 1.39 1.60 2.97 Acceptable 2.9% Acceptable Acceptable137Cs 03 2.6 0.2 3.2 0.2 6.9% 21% 2.10 1.85 0.55 0.77 Acceptable 10.3% Acceptable Acceptable137Cs 04 38.4 0.8 38.6 0.8 2.1% 0% 0.04 0.12 0.14 2.97 Acceptable 3.0% Acceptable Acceptable137Cs 05 20.3 0.5 20.9 1.0 4.8% 3% 0.28 0.50 0.56 2.88 Acceptable 5.4% Acceptable Acceptable

1.001.03

1.041.21

Samplecode

LaboratoryLab./IAEA

1.03

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Page 47

Analytical Performance Evaluation of Laboratory 17137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 20.95 0.46 2.2% 3% 0.32 0.95 0.64 1.75 Acceptable 3.3% Acceptable Acceptable210Pb 01 289.0 7.0 290 16 5.5% 0% 0.03 0.06 1.00 45.06 Acceptable 6.0% Acceptable Acceptable137Cs 02 38.4 0.8 43.13 0.79 1.8% 12% 1.23 4.13 4.73 2.96 Not Acceptable 2.8% Acceptable Warning210Pb 02 530.0 11.3 543 24 4.4% 2% 0.25 0.49 13.00 68.44 Acceptable 4.9% Acceptable Acceptable137Cs 03 2.6 0.2 2.83 0.23 8.1% 8% 0.80 0.69 0.21 0.79 Acceptable 11.2% Acceptable Acceptable210Pb 03 48.0 1.5 48 9 18.8% 0% 0.00 0.00 0.00 23.54 Acceptable 19.0% Acceptable Acceptable137Cs 04 38.4 0.8 43.40 0.79 1.8% 13% 1.29 4.35 4.98 2.95 Not Acceptable 2.8% Acceptable Warning210Pb 04 530.0 11.3 557 25 4.5% 5% 0.51 0.98 27.00 70.78 Acceptable 5.0% Acceptable Acceptable137Cs 05 20.3 0.5 21.01 0.62 3.0% 3% 0.35 0.89 0.71 2.05 Acceptable 3.8% Acceptable Acceptable210Pb 05 289.0 7.0 250 16 6.4% -13% -1.35 -2.23 39.00 45.04 Acceptable 6.8% Acceptable Acceptable0.87

1.001.131.051.03

1.001.121.021.08

Samplecode

LaboratoryLab./IAEA

1.03

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Page 48 48

Analytical Performance Evaluation of Laboratory 18137Cs and 210Pb in spiked soil

Reference date: 1 - 01- 2006IAEA Acceptance criteria

Analyte Value Unc. Value Unc. R. bias Z-score U-Test Trueness Precision Final score[Bq/kg] [Bq/kg] [Bq/kg] [Bq/kg] % % A1 A2 Score P Score

137Cs 01 20.3 0.5 19.9 0.8 4.0% -2% -0.20 -0.43 0.41 2.43 Acceptable 4.7% Acceptable Acceptable210Pb 01 289.0 7.0 316.5 17.3 5.5% 10% 0.95 1.47 27.50 48.15 Acceptable 6.0% Acceptable Acceptable137Cs 02 38.4 0.8 40.5 1.3 3.2% 5% 0.55 1.36 2.10 3.98 Acceptable 3.9% Acceptable Acceptable210Pb 02 530.0 11.3 602.1 31.4 5.2% 14% 1.36 2.16 72.10 86.10 Acceptable 5.6% Acceptable Acceptable137Cs 03 2.6 0.2 2.5 0.3 12.0% -5% -0.46 -0.33 0.12 0.93 Acceptable 14.2% Acceptable Acceptable210Pb 03 48.0 1.5 64.1 4.0 6.2% 34% 3.35 3.77 16.10 11.02 Not Acceptable 7.0% Acceptable Not Acceptable137Cs 04 38.4 0.8 39.9 1.2 3.0% 4% 0.38 1.01 1.48 3.76 Acceptable 3.7% Acceptable Acceptable210Pb 04 530.0 11.3 599.0 32.6 5.4% 13% 1.30 2.00 69.00 89.02 Acceptable 5.8% Acceptable Acceptable137Cs 05 20.3 0.5 20.3 0.8 3.9% 0% 0.00 0.00 0.00 2.43 Acceptable 4.6% Acceptable Acceptable210Pb 05 289.0 7.0 310.4 18.1 5.8% 7% 0.74 1.10 21.40 50.05 Acceptable 6.3% Acceptable Acceptable1.07

1.341.041.131.00

1.101.051.140.95

Samplecode

LaboratoryLab./IAEA

0.98

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Page 49

Appendix C: List of Participants

Dr. Alfonso Bujan Div. De Aplicaciones Agropecuarias Comision Nacional De Energia Atomica Av. Del Liberator 8250 1429, Buenos Aires Argentina

Dr. Chris Leslie C.S.I.R.O. Clunies Ross Street P.O. Box 1666 Canberra, A.C.T. 2601 Australia

Mr. John Pfitzner Coastal Process Group Australian Institute Of Marine Science Pmb 3, Mail Centre Townsville, Mc 4810 Australia

Dr. Osny Oliveira Bacchi Soils Physics Section Centre Of Nuclear Energy In The Agriculture University Of Sao Paulo Av. Centenario, 303 Cp 96 Cep 13400-970, Piracicaba, , Sao Paulo Brazil

Dr. David Lobb Department Of Soil Science University Of Manitoba Winnipeg, R3t 2n2 Canada

Dr. Yong Li Institute Of Agricultural Environment And Sustainable Development Chinese Academy Of Agricultural Sciences No. 12 Zhongguancun South Street 100 094, Beijing, 100081 China

Prof. Paulina Schuller Liewald Laboratorio Radioecologia Instituto De Fisica, Facultad De Ciencias Universidad Austral De Chile Independencia 641 P.O. Box (Casilla) 567 Valdivia Chile

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Page 50 50

Prof. Xinbao Zhang Institute Of Mountain Hazards And Environment Academy Of Sciences And Ministry Of Water Resources No. 4 Block, Renminnanlu/No. 9 P.O. Box 417 Chengdu, 610041 Sichuan China

Dr. Yuichi Onda Institute Of Geoscience University Of Tsukuba Ibaraki, 305-8571 Tsukuba Japan

Dr. Moncef Benmansour Departement Des Applications Aux Sciences De La Terre Et De L Environnement Centre National De L'energie Des Sciences Et Des Techniques Nucleaires (Cnesten) 65 Rue Tansift- Agdal Rabat Morocco

Dr. Muhammad Rafiq Sheikh Radiation And Isotope Applications Div. Pakistan Institute Of Nuclear Science & Technology (Pinstech) Mnsr Lab. Naa Acg P.O.Box 1114, Nilore 92/051, Islamabad Pakistan

Prof. Wojciech Froehlich Homerka Laboratory Of Fluvial Processes Institute Of Geography And Spatial Organization Polish Academy Of Sciences Frycowa 113 P.O.Box 2 Pl-33-335, Nawojowa Poland

Dr. Nelu Popa Central Research Station For Soil Erosion Control P.O.Box 1 R-6400, Perieni Barlad Romania

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Page 51

Dr. Valentin Golosov Laboratory For Soil Erosion And Fluvial Processes Department Of Geography Lomonosov Moscow State University Leninskie Gory 119992, Gsp-2, Moscow Russian Federation

Dr. Sevilay Haciyakupoglu Institute Of Energy Nuclear Research Department Istanbul Technical Univesity Maslak 34390, Maslak, Istanbul Turkey

Dr. Desmond E. Walling Department Of Geography University Of Exeter Amory Building, Rennes Drive Exeter, Ex4 4rj Devon United Kingdom

Dr. Jerry C. Ritchie Hydrology And Remote Sensing Laboratory Barc-West Bldg-007 Usda Agriculture Research Service 13300 Baltimore Avenue Beltsville, Md 20705 United States Of America

Mr. Son Hai Phan Sedimentology Laboratory Viet Nam Atomic Energy Commission Nuclear Research Institute 01 Nguyen Tu Luc Street 61 100, Dalat Viet Nam