ELEMENTS IN SOIL PROFICIENCY TESTING REPORT
Report No: KAR-G3RM-420.2018.01 (Rev. 02)
Prepared by: Dr. Fatma AKÇADAĞ
TÜBİTAK UME Reference Materials Laboratory
27.08.2018 Gebze-KOCAELI/TURKEY ULUSAL METROLOJİ ENSTİTÜSÜ TÜBİTAK Gebze Yerleşkesi P.K. 54, 41470 Gebze Kocaeli T 0 262 679 50 00 F 0 262 679 50 01 www.ume.tubitak.gov.tr
Elements in Soil Proficiency Testing Report
This proficiency testing was carried out by TÜBİTAK UME Reference Materials Laboratory (Turkey), Jožef Stefan Institute (IJS) (Slovenia) and Institute of Metrology of B&H (IMBIH) (Bosnia and Herzegovina) in accordance with the “ISO/IEC 17043: 2010 Conformity Assessment - General Requirements for Proficiency Testing”
TÜBİTAK Ulusal Metroloji Enstitüsü (UME) Referans Malzemeler Laboratuvarı P.K. 54 41470 Gebze KOCAELİ/TURKEY Phone: 0 262 679 50 00 ext. 6400 or 6209; Fax: 0 262 679 50 01 www.ume.tubitak.gov.tr
Coordinator Dr. Fatma AKÇADAĞ e-mail:
[email protected]
Scheme Coorganizers Milena HORVAT, Radojko JACIMOVIC, Jožef Stefan Institute (IJS), SLOVENIA Aida JOTANOVIC, IMBIH (Metrology Institute), BOSNIA and HERZEGOVINA
Dr. Alper İŞLEYEN Head of Reference Materials Laboratory
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Elements in Soil Proficiency Testing Report
CONTENT
1.
INTRODUCTION ................................................................................................................. 6
2.
ORGANISATION AND DESIGN .......................................................................................... 7
3.
PARTICIPATIONS............................................................................................................... 7
4.
INSTRUCTIONS TO THE PARTICIPANTS ......................................................................... 7
5.
TEST MATERIAL ................................................................................................................ 8
6.
METHODS AND INSTRUMENTATION USED .................................................................... 8
7.
REPORTING RESULTS ...................................................................................................... 8
8.
CONFIDENTIALITY........................................................................................................... 17
9.
RESULTS AND EVALUATION OF THE PERFORMANCE ................................................ 17
10. REMARK AND COMMENTS ............................................................................................. 50 11. ACKNOWLEDGEMENTS .................................................................................................. 50 12. REFERENCES .................................................................................................................. 50
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TABLES Table 1. Methods used by the participants ............................................................................. 9 Table 2. Instruments used by the participants ...................................................................... 13 Table 3. Participant’s results for As, B and Cd in soil ............................................................ 19 Table 4. Participant’s results for Co, Cu and Pb in soil ......................................................... 20 Table 5. Participant’s results for Sb, Zn and Ca in soil .......................................................... 21 Table 6. Participant’s results for Cr, Fe and Mg in soil .......................................................... 22 Table 7. Participant’s results for Mn, Ni and Al in soil ........................................................... 23 Table 8. Participant’s results for Ba, V, Hg and mositure in soil ............................................ 24 Table 9. Participant’s results and z score for aqua regia extractable content of As, B, Cd and Co in soil .............................................................................................................................. 25 Table 10. Participant’s results and z score for aqua regia extractable content of Cu, Pb, Sb and Zn in soil ........................................................................................................................ 26 Table 11. Participant’s results and z score for aqua regia extractable content of Ca, Cr, Fe and Mg in soil ....................................................................................................................... 27 Table 12. Participant’s results and z score for aqua regia extractable content of Mn, Ni, Al and Ba in soil........................................................................................................................ 28 Table 13. Participant’s results and z score for aqua regia extractable content of V, Hg and moisture in soil ..................................................................................................................... 29 Table 14. Participant’s results and z score for total content of As, B, Cd and Co in soil ........ 30 Table 15. Participant’s results and z score for total content of Cu, Pb, Sb and Zn in soil ...... 31 Table 16. Participant’s results and z score for total content of Ca, Cr, Fe and Mg in soil ...... 32 Table 17. Participant’s results and z score for total content of Mn, Ni, Al and Ba in soil ........ 33 Table 18. Participant’s results and z score for total content of V, Hg and moisture in soil ..... 34 Table 19. Distribution of the z scores for aqua regia extractable content of elements in soil . 44 Table 20. Distribution of the z scores for total content of elements in soil ............................. 45 Table 21. Distribution of the results for aqua regia extractable content of As, B, Cd, Co, Cu, Pb, Sb, Zn, Ba, V, Cr, Mn, Ni and Hg in soil ......................................................................... 46 Table 22. Distribution of the results for aqua regia extractable content of Al, Ca, Fe, Mg and moisture in soil ..................................................................................................................... 47 Table 23. Distribution of the results for total content of As, B, Cd, Co, Cu, Pb, Sb, Zn, Ba, V, Cr, Mn, Ni and Hg in soil....................................................................................................... 48 Table 24. Distribution of the results for total content of Al, Ca, Fe, Mg and moisture in soil .. 49
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Toprakta Element Tayini Yeterlilik Testi Raporu
FIGURES Figure 1. Participant’s z scores for aqua regia extractable content of As in soil ........................ 35 Figure 2. Participant’s z scores for aqua regia extractable content of B in soil .......................... 35 Figure 3. Participant’s z scores for aqua regia extractable content of Cd in soil ........................ 35 Figure 4. Participant’s z scores for aqua regia extractable content of Co in soil ........................ 35 Figure 5. Participant’s z scores for aqua regia extractable content of Cu in soil ........................ 36 Figure 6. Participant’s z scores for aqua regia extractable content of Pb in soil ........................ 36 Figure 7. Participant’s z scores for aqua regia extractable content of Sb in soil ........................ 36 Figure 8. Participant’s z scores for aqua regia extractable content of Zn in soil ........................ 36 Figure 9. Participant’s z scores for aqua regia extractable content of Ca in soil ........................ 37 Figure 10. Participant’s z scores for aqua regia extractable content of Cr in soil ...................... 37 Figure 11. Participant’s z scores for aqua regia extractable content of Fe in soil ...................... 37 Figure 12. Participant’s z scores for aqua regia extractable content of Mg in soil ..................... 37 Figure 13. Participant’s z scores for aqua regia extractable content of Mn in soil ..................... 38 Figure 14. Participant’s z scores for aqua regia extractable content of Ni in soil ....................... 38 Figure 15. Participant’s z scores for aqua regia extractable content of Al in soil ....................... 38 Figure 16. Participant’s z scores for aqua regia extractable content of Ba in soil ...................... 38 Figure 17. Participant’s z scores for aqua regia extractable content of V in soil ........................ 39 Figure 18. Participant’s z scores for aqua regia extractable content of Hg in soil ...................... 39 Figure 19. Participant’s z scores for total content of As in soil .................................................. 39 Figure 20. Participant’s z scores for total content of B in soil .................................................... 39 Figure 21. Participant’s z scores for total content of Cd in soil .................................................. 40 Figure 22. Participant’s z scores for total content of Co in soil .................................................. 40 Figure 23. Participant’s z scores for total content of Cu in soil .................................................. 40 Figure 24. Participant’s z scores for total content of Pb in soil .................................................. 40 Figure 25. Participant’s z scores for total content of Sb in soil .................................................. 41 Figure 26. Participant’s z scores for total content of Zn in soil .................................................. 41 Figure 27. Participant’s z scores for total content of Ca in soil .................................................. 41 Figure 28. Participant’s z scores for total content of Cr in soil ................................................... 41 Figure 29. Participant’s z scores for total content of Fe in soil .................................................. 42 Figure 30. Participant’s z scores for total content of Mg in soil.................................................. 42 Figure 31. Participant’s z scores for total content of Mn in soil.................................................. 42 Figure 32. Participant’s z scores for total content of Ni in soil ................................................... 42 Figure 33. Participant’s z scores for total content of Al in soil ................................................... 43 Figure 34. Participant’s z scores for total content of Ba in soil .................................................. 43 Figure 35. Participant’s z scores for total content of V in soil .................................................... 43 Figure 36. Participant’s z scores for total content of Hg in soil .................................................. 43 v / 50
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Elements in Soil Proficiency Testing Report
1. INTRODUCTION
Proficiency testing (PT) is defined in ISO/IEC 17043: 2010 as the use of inter-laboratory comparisons to determine the performance of individual laboratories for specific tests or measurements and to monitor laboratories’ continuing performance.
When performed within the context of a comprehensive quality assurance programme, proficiency testing is an independent means of assuring the quality of test and calibration results, as described in ISO/IEC17025 laboratory’s participation in proficiency testing activities is requirement of the standard. The purpose of this requirement is to provide interested parties with objective evidence of a laboratory’s capability to produce data that is both accurate and repeatable for activities listed in its competence to cl ients, potential customers, accreditation bodies and other external entities. Participation in proficiency testing activities also provide in valuable feedback in the internal monitoring of a laboratory’s quality system. Trough these activities, a laboratory can verify its competence to perform specific calibrations of tests.
In this PT study, participants were asked to measure the amount of elements As, B, Cd, Co, Cu, Pb, Sb, Zn, Ca, Cr, Fe, Mg, Mn, Ni, Al, Ba, V and Hg in soil. This Proficiency Testing scheme operated in accordance with ISO/IEC 17043: 2010 The aim of this study is to determine the performances of the laboratories that analysis elements (As, B, Cd, Co, Cu, Pb, Sb, Zn, Ca, Cr, Fe, Mg, Mn, Ni, Al, Ba, V and Hg) in soil and contribute to improving their performance.
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2. ORGANISATION AND DESIGN
Scheme Coordinator The day-to-day operation of scheme is the responsibility of Scheme Coordinator. Coordinator: Dr. Fatma AKÇADAĞ, TUBITAK UME (National Metrology Institute), TURKEY
Scheme Coorganizers Milena HORVAT, Radojko JACIMOVIC, Jozef Stefan Institute (IJS), SLOVENIA Aida JOTANOVIC, IMBIH (Metrology Institute), BOSNIA&HERZEGOVINA Technical Group Technical group consists of members who ar e experienced in the field of the preparation and test. Technical Group: Fatma AKÇADAĞ, Alper İŞLEYEN, Oktay CANKUR, Milena HORVAT, Radojko JACIMOVIC and Aida JOTANOVIC.
Scheme coordinator and technical group are responsible for preparation of test materials, testing of reference materials, evaluation of results, reporting, and dealing with technical issues. 3. PARTICIPATIONS
Proficiency testing scheme is open to all laboratories in the field. Fifteen laboratories from Bosnia and Herzegovina, Finland, Slovenia and Turkey (except UME and IJS) were participated to this PT scheme. 4. INSTRUCTIONS TO THE PARTICIPANTS
A technical protocol was sent to all participants of the PT, at the same date of the sample distribution providing information concerning the samples, sample storage, the recommended measurement method and confidentiality. Additionally a report form was distributed for reporting the results and additional information requested from the participants.
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5. TEST MATERIAL Candidate soil certified reference material (CRM) produced within the scope of ENVCRM project (www.envcrm.com) was used as the test material in this PT scheme. A soil sample obtained from Çayırhan (Ankara, Turkey) thermal power plant district was used. Test sample was prepared by blending contaminated soil [spiked with elements (Cd, Co, Cu, Hg, Ni, Pb, Sb and Zn) which was dried, milled, sieved soil (< 90 µm) and homogenized] and natural soil [which was also dried, milled, sieved (< 100 µm) and homogenized]. The soil blend was then further homogenized for 12 h and filled in to amber glass bottles as 25 g. The bottles were then sterilised by
Co -irradiation with 25 kGy dose. All samples were sent to participants at the
60
same time by courier in 2018-04-16. A technical protocol including the purpose of the work, the organizers, the conditions for participation in the work, the information about the test sample, the work schedule, the parameters to be determined, the methods to be used, the reporting of the results and the confidentiality of the work was sent to the participating laboratories by e-mail at the same date of the sample distribution. Technical protocol was also published on TÜBİTAK UME website for Turkish the participants in Turkish. Participating laboratories were asked to conduct their work in accordance with this protocol. The participating laboratories were asked to report their results with
corresponding
measurement
uncertainties,
standard
deviation
values,
and
the
methods/instruments they used during the analysis. 6. METHODS AND INSTRUMENTATION USED Participants were free to use a method of their choice. It was recommended to use the same method and operator with routine analyses. Participants were asked to treat the PT material in the same way as a routine sample, and to state their method and instrument when reporting results. Results were evaluated according to the methods used by participants. Methods applied and instrumentations used in the analysis by the participants are given in the Table 1 and Table 2. 7. REPORTING RESULTS Participants were asked to report their results on dry basis and specify the information that the reported results either total content (T) or aqua regia extractable content (E) of elements in soil. Participants from Turkey reported their results by using company ID and password in https://interaktif.ume.tubitak.gov.tr/yt website. Other participants reported their results by using “Elements in Soil Report Form”. 8 / 50
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Table 1. Methods used by the participants Lab. Code
As
B
Cd
Co
Cu
01-a
-
EPA 6020 A
-
-
-
01-b
-
EN ISO 11885
-
-
-
02
-
-
-
-
In House Method
03
In House Method
-
In House Method
In House Method
In House Method
04
-
05
-
-
-
-
-
06
-
-
-
EPA 6010 C
EPA 6010 C
07
-
TS EN 13650
TS EN 13650
TS EN 13650
TS EN 13650
08
-
-
-
-
-
09
-
-
Microw ave digestion
Microw ave digestion
Microw ave digestion
10
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
11
EPA 3050 B TS EN EPA 3050 B TS EN EPA 3050 B TS EN EPA 3050 B TS EN ISO 11885 ISO 11885 ISO 11885 ISO 11885
SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885
12
SFS-EN 16171:2016
SFS-EN 16171:2016
SFS-EN 16171:2016
SFS-EN 16171:2016
SFS-EN 16171:2016
13
EN 16170:2016
EN 16170:2016
EN 16170:2016
EN 16170:2016
EN 16170:2016
14
BAS ISO 11047:2000
-
BAS ISO 11047:2000
BAS ISO 11047:2000
BAS ISO 11047:2000
15
In House Method
-
In House Method
In House Method
In House Method
IJS
-
-
-
-
-
UME
-
-
-
-
-
ENVCRM-T
-
-
-
-
-
-
ISO 12914: 2012, ISO 11466: 1995, ISO 16965: 2013
ISO 12914: 2012, ISO 11466: 1995, ISO 16965: 2013
ISO 12914: 2012
ISO 12914: 2012, ENVCRM-E ISO 11466: 1995, ISO 16965: 2013
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Table 1. Methods used by the participants (continue) Lab. Code
Pb
Sb
Zn
Ca
Cr
01-a
-
EPA 6020 A
EN ISO 11885
-
-
01-b
-
EPA 6020 A
EN ISO 11885
-
-
02
In House Method
-
In House Method
-
In House Method
03
In House Method
-
In House Method
-
In House Method
04
EPA 3050 B TS EN ISO 11885
-
EPA 3050 B TS EN ISO 11885
-
EPA 3050 B TS EN ISO 11885
05
-
-
-
-
-
06
-
-
-
-
EPA 6010 C
07
TS EN 13650
-
TS EN 13650
TS EN 13650
TS EN 13650
08
-
-
-
-
EPA 3051 A - SM 3125 B
09
Microw ave digestion
-
Microw ave digestion
Microw ave digestion
Microw ave digestion
10
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
11
SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885
12
SFS-EN 16171:2016
SFS-EN 16171:2016
SFS-EN 16171:2016
SFS-EN 16170:2016
SFS-EN 16171:2016
13
EN 16170:2016
EN 16170:2016
EN 16170:2016
EN 16170:2016
EN 16170:2016
14
BAS ISO 11047:2000
-
BAS ISO 11047:2000
BAS ISO 11466:2000
-
15
In House Method
In House Method
In House Method
In House Method
In House Method
IJS
-
-
-
-
-
UME
-
-
-
-
-
ENVCRM-T
-
-
-
-
-
ISO 12914: 2012, ISO 11466: 1995, ISO 16965: 2013
ISO 12914: 2012, ISO 11466: 1995, ISO 16965: 2013
-
ISO 12914: 2012, ISO 11466: 1995, ISO 16965: 2013
ISO 12914: 2012, ENVCRM-E ISO 11466: 1995, ISO 16965: 2013
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Table 1. Methods used by the participants (continue)
Lab. Code
Fe
Mg
Mn
Ni
Al
01-a
-
-
-
-
-
01-b
-
-
-
-
-
02
In House Method
-
-
-
-
03
-
-
In House Method
In House Method
-
04
EPA 3050 B TS EN ISO 11885
-
05
EPA 200.7
-
-
-
-
06
-
-
-
-
-
07
TS EN 13650
TS EN 13650
TS EN 13650
TS EN 13650
TS EN 13650
08
EPA 3051 A - SM 3125 B
-
EPA 3051 A - SM 3125 B
-
EPA 3051 A - SM 3125 B
09
Microw ave digestion
Microw ave digestion
Microw ave digestion
Microw ave digestion
-
10
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
11
EPA 3050 B TS EN EPA 3050 B TS EN ISO 11885 ISO 11885
-
SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885 SFS-EN ISO 11885
12
SFS-EN 16170:2016
SFS-EN 16170:2016
SFS-EN 16171:2016
SFS-EN 16171:2016
SFS-EN 16170:2016
13
EN 16170:2016
EN 16170:2016
EN 16170:2016
EN 16170:2016
EN 16170:2016
14
BAS ISO 11466:2000
BAS ISO 11466:2000
BAS ISO 11047:2000
BAS ISO 11047:2000
-
15
In House Method
In House Method
In House Method
In House Method
In House Method
IJS
-
-
-
-
-
UME
-
-
-
-
-
ENVCRM-T
-
-
-
-
-
ENVCRM-E
ISO 11466: 1995, ISO 16965: 2013
-
ISO 11466: 1995, ISO 16965: 2013
ISO 12914: 2012, ISO 11466: 1995, ISO 16965: 2013
-
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Table 1. Methods used by the participants (continue)
Lab. Code
Ba
V
Hg
Moisture
01-a
-
-
-
TS 9546 EN 12880
01-b
-
-
-
TS 9546 EN 12880
02
In House Method
-
-
-
03
-
-
-
-
04
-
-
-
-
05
-
-
-
-
06
EPA 6010 C
-
-
TS 9546 EN 12880
07
TS EN 13650
-
-
ISO 11465
08
EPA 3051 A - SM 3125 B
-
EPA 3051 A - SM 3125 B
EPA 3051 A
09
-
-
-
Tüzüner, 1990
10
TS EN 13656, TS EN ISO 11885
TS EN 13656, TS EN ISO 11885
11
TS EN 13656, In House MethodTS 9546 EN 12880 DPP_TLL_Ç19.Rev.02 ( TS EN ISO 11885)
SFS-EN ISO 11885 SFS-EN ISO 11885
ISO 16772
ISO 11465 SFS 3008:1990
12
SFS-EN 16170:2016
SFS-EN 16171:2016
SFS-EN 16171:2016
13
EN 16170:2016
EN 16170:2016
EN 16170:2016
14
-
-
Direct by thermal decomposition,gold am.
15
-
-
In House Method
Gravimetric
IJS
-
-
-
-
UME
-
-
-
ISO 11465
ENVCRM-T
-
-
-
-
ENVCRM-E
-
ISO 12914: 2012
ISO 12914: 2012
-
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SIST EN 14346:2007 method A BAS ISO 11465:2000
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Table 2. Instruments used by the participants
Lab. Code
As
B
Cd
Co
Cu
01-a
-
ICP-MS
-
-
-
01-b
-
ICP-OES
-
-
-
02
-
-
-
-
ICP-OES
03
ICP-MS
-
ICP-MS
ICP-MS
ICP-MS
04
-
ICP-OES
ICP-OES
ICP-OES
ICP-OES
05
-
-
-
-
-
06
-
-
-
ICP-OES
ICP-OES
07
-
ICP-OES
ICP-OES
ICP-OES
ICP-OES
08
-
-
-
-
-
09
-
-
ICP-OES
ICP-OES
ICP-OES
10
ICP-OES
ICP-OES
ICP-OES
ICP-OES
ICP-OES
11
ICP-OES
ICP-OES
ICP-OES
ICP-OES
ICP-OES
12
ICP-MS
ICP-MS
ICP-MS
ICP-MS
ICP-MS
13
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
14
AAS-Hydride technique
-
GFAAS
FAAS
FAAS
15
EAAS
-
EAAS
EAAS
EAAS
IJS
-
-
-
-
-
UME
-
ICP-MS
-
-
-
ENVCRM-T
k0-INAA (TRIGA rector and HPGe detector)
-
ID-ICP-MS
ENVCRM-E
ICP-MS, ICP OES
-
ICP-MS, ASV
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ICP-MS
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Table 2. Instruments used by the participants (continue) Lab. Code
Pb
Sb
Zn
Ca
Cr
01-a
-
ICP-MS
ICP-OES
-
-
01-b
-
ICP-MS
ICP-OES
-
-
02
ICP-OES
-
ICP-OES
-
ICP-OES
03
ICP-MS
-
ICP-MS
-
ICP-MS
04
ICP-OES
-
ICP-OES
-
ICP-OES
05
-
-
-
-
-
06
-
-
-
-
ICP-OES
07
ICP-OES
-
ICP-OES
ICP-OES
ICP-OES
08
-
-
-
-
ICP-MS
09
ICP-OES
-
ICP-OES
ICP-OES
ICP-OES
10
ICP-OES
ICP-OES
ICP-OES
ICP-OES
ICP-OES
11
ICP-OES
ICP-OES
ICP-OES
ICP-OES
ICP-OES
12
ICP-MS
ICP-MS
ICP-MS
ICP-OES
ICP-MS
13
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
14
FAAS
-
FAAS
FAAS
-
15
FAAS
EAAS
FAAS
FAAS
EAAS
IJS
-
-
-
k0-INAA (TRIGA rector and HPGe detector)
-
UME
-
-
-
-
-
ENVCRM-T
ID-ICP-MS
k0-INAA (TRIGA rector and HPGe detector)
-
k0-INAA, ID-ICPMS
ENVCRM-E
ICP-MS, ICP-OES, ASV
ICP-MS
k0-INAA, ID-ICPMS, ICP-MS, ICPOES, MPAES ICP-MS, ICP-OES, ASV
-
ICP-MS, ICP-OES
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Table 2. Instruments used by the participants (continue) Lab. Code
Fe
Mg
Mn
Ni
Al
01-a
-
-
-
-
-
01-b
-
-
-
-
-
02
ICP-OES
-
-
-
-
03
-
-
ICP-MS
ICP-MS
-
04
ICP-OES
-
ICP-OES
ICP-OES
-
05
ICP-OES
-
-
-
-
06
-
-
-
-
-
07
ICP-OES
ICP-OES
ICP-OES
ICP-OES
ICP-OES
08
ICP-MS
-
ICP-MS
-
ICP-MS
09
ICP-OES
ICP-OES
ICP-OES
ICP-OES
-
10
ICP-OES
ICP-OES
ICP-OES
ICP-OES
ICP-OES
11
ICP-OES
ICP-OES
ICP-OES
ICP-OES
ICP-OES
12
ICP-OES
ICP-OES
ICP-MS
ICP-MS
ICP-OES
13
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP OES Spectro Ciros Vision
ICP-OES
ICP-OES
14
FAAS
FAAS
FAAS
FAAS
-
15
FAAS
FAAS
FAAS
FAAS
FAAS
IJS
-
k0-INAA (TRIGA rector and HPGe detector)
-
-
k0-INAA (TRIGA rector and HPGe detector)
UME
-
-
-
-
-
ENVCRM-T
k0-INAA, ID-ICPMS, ICPMS,MPAES, AAS
-
ENVCRM-E
ICP-MS
-
k0-INAA, ICP-MS, MP- ID-ICP-MS, ICP-MS, AES ICP-OESMP-AES ICP-MS
15 / 50
ICP-MS, ICP-OES
-
-
Rev. 02/27.08.2018
Elements in Soil Proficiency Testing Report
Table 2. Instruments used by the participants (continue) Lab. Code
Ba
V
Hg
Moisture
01-a
-
-
-
-
01-b
-
-
-
-
02
ICP-OES
-
-
-
03
-
-
-
-
04
-
-
-
-
05
-
-
-
-
06
ICP-OES
-
-
-
07
ICP-OES
-
-
-
08
ICP-MS
-
ICP-MS
-
09
-
-
-
-
10
ICP-OES
ICP-OES
ICP-OES
-
11
ICP-OES
ICP-OES
CVAAS
105 °C, 16 h
12
ICP-OES
ICP-MS
ICP-MS
105 °C, 24 h
13
ICP-OES
ICP-OES
ICP-OES
105 °C, 2 h
14
-
-
SMS Solid mercury system
4 hours, 105 °C
15
-
-
AMA
105 °C
IJS
k0-INAA (TRIGA rector and HPGe detector)
-
-
Oven, Balance (103 ± 2) °C
UME
-
-
-
Oven, Balance (103 ± 2) °C
ENVCRM-T
-
k0-INAA, ICP-MS, ICPOES, MP-AES
ID-ICP-MS
-
ENVCRM-E
-
ICP-MS
ICP-MS
-
16 / 50
Rev. 02/27.08.2018
Elements in Soil Proficiency Testing Report
8. CONFIDENTIALITY In order to ensure confidentiality, each participant in the scheme is allocated with a unique laboratory code. This number enables results to be reported without reveal the identities of participant laboratories. All information supplied by a participant to the proficiency testing provider treated as confidential. 9. RESULTS AND EVALUATION OF THE PERFORMANCE In this PT scheme, participants were asked to report the results as either aqua regia extractable content of elements or total content of elements. The results were evaluated separately in terms of aqua regia extractable content of elements and total content of elements. Assigned values for aqua regia extractable content of elements were determined by median of the participant results. The assigned values for the results reported as total elements (except Al, B, Ba, Ca and Mg) content were determined by the project consortium who produced the candidate certified reference material (www.envcrm.com). Assigned values for total Al, Ba, Ca and Mg were determined by IJS with k0-INAA method. Assigned value for B was determined by TUBITAK UME with ICP-MS.
Standard deviations for proficiency testing assessment (σpt) were determined as different percent of reference values depending on the parameters and previous experience in this area. Standard deviation for Sb was determined as 25 % of the assigned value and for the other elements it was determined as 20 % of the assigned values. Participants’ z scores were calculated using the following equation;
z
x X pt σ pt
where; x = participant’s result Xpt = assigned value σpt = standard deviation for proficiency testing assessment (SDPA)
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Rev. 02/27.08.2018
Elements in Soil Proficiency Testing Report
For z score the following interpretation is given to results. |z| ≤ 2.0
satisfactory result
2.0 < |z| < 3.0
questionable result
|z| ≥ 3.0
unsatisfactory result
All the participants’ results are given in Table 3 to Table 8. In these tables results reported by the laboratories as aqua regia extractable element content were specified as (E) and results reported as total element content were specified as (T) and indicated in a separate column. Evaluated results reported by participants as aqua regia extractable element content are given in Table 9 to Table 13, and as total elements in Table 14 to Table 18.
Graphical representations of z scores for the results reported as aqua regia extractable element content are provided in Figure 1 to Figure 18, and for the results reported as total element content in Figures 19 to 36.
Distribution of the z scores for the results reported as aqua regia extractable element content and total element content are given in Table 19 to Table 20, respectively. Distribution of the results reported as aqua regia extractable element content are given in Table 21 to Table 23 and total element content in Table 24 to Table 26.
The participants 2, 10, 11, 12, 13, 14 and 15 have reported measurement uncertainty for k = 2. Measurement uncertainty values of laboratory coded 12 are reported as %.
18 / 50
Rev. 02/27.08.2018
Elements in Soil Proficiency Testing Report
Table 3. Participant’s results for As, B and Cd in soil
Lab. Code
As
B
Cd
mg/kg
mg/kg
mg/kg
E/T
Result
s
Uncertainty
Result
s
Uncertainty
Result
s
Uncertainty
01-a
-
-
-
123.01
-
-
-
-
-
T
01-b
-
-
-
129.8
-
-
-
-
-
T
02
-
-
-
-
-
-
-
-
-
-
03
69.9
-
-
-
-
-
1.55
-
-
E
04
-
-
-
124
-
-
3.58
-
-
E
05
-
-
-
-
-
-
-
-
-
T
06
-
-
-
-
-
-
-
-
-
E
07
-
-
-
67.92
-
-
0.461
-
-
E
08
-
-
-
-
-
-
-
-
-
-
09
-
-
-
-
-
-
0.54
-
-
E
10
60.52
-
2.9
196.76
-
-
1.07
-
0.05
T
11
67.1
0.64
11.4
108
1.1
18
1.08
0.02
0.19
E
12*
68
1.7
20
124
5.6
20
1.02
0.002
20
E
13
59.62
0.66
2.98
124.75
2.34
6.24
1.25
0.16
0.06
E
14
62.48
0.98
-
-
-
-
0.81
0.077
0.1
E
15
90.54
8.69
15
-
-
-
0.140
0.010
10
T
IJS
-
-
-
-
-
-
-
-
-
-
UME
-
-
-
148.6
1.7
-
-
-
-
T
ENVCRM-T
79.94
0.77
-
-
-
-
1.292
0.005
-
T
ENVCRM-E
70.25
1.06
-
-
-
-
1.292
0.094
-
E
* Measurement uncertainty is reported as %. 19 / 50
Rev. 02/27.08.2018
Elements in Soil Proficiency Testing Report
Table 4. Participant’s results for Co, Cu and Pb in soil
Lab. Code
Co
Cu
Pb
mg/kg
mg/kg
mg/kg
E/T
Result
s
Uncertainty
Result
s
Uncertainty
Result
s
Uncertainty
-
-
-
-
-
-
-
-
-
-
01-b
-
-
-
-
-
-
-
-
-
-
02
-
-
-
60.85
0.56
2.6
41.0
0.4
2.5
E
03
43.61
-
-
56.02
-
-
55.7
-
-
E
04
33.66
-
-
64.7
-
-
48.0
-
-
E
05
-
-
-
-
-
-
-
-
-
-
06
42.84
-
-
68.67
-
-
-
-
-
E
07
35.87
-
-
51.97
-
-
32.3
-
-
E
08
-
-
-
-
-
-
-
-
-
-
09
25.42
-
-
44.8
-
-
31.4
-
-
E
10
34.53
-
-
52.48
-
2.92
57.9
-
2.7
T
11
37.7
0.4
6
60.5
2.1
9.1
51.0
1.0
9.2
E
12*
40.2
0.63
20
58.2
1.4
20
57.1
1.3
20
E
13
36.44
0.36
1.82
51.24
0.54
2.56
41.33
2.04
3.2
E
14
30.1
0.004
5.13
59.4
0.02
6.76
62.6
0.0
6.1
E
15
34.46
3.96
10
59.01
1.28
10
69.11
2.46
10
T
IJS
-
-
-
-
-
-
-
-
-
-
UME
-
-
-
-
-
-
-
-
-
-
ENVCRM-T
42.04
0.63
-
63.52
1.49
-
64.14
0.06
-
T
ENVCRM-E
41.73
3.16
-
63.0
5.4
-
63.1
11.6
-
E
* Measurement uncertainties are reported as %. 20 / 50
Rev. 02/27.08.2018
Elements in Soil Proficiency Testing Report
Table 5. Participant’s results for Sb, Zn and Ca in soil
Lab. Code
Sb
Zn
Ca
mg/kg
mg/kg
g/kg
E/T
Result
s
Uncertainty
Result
s
Uncertainty
Result
s
Uncertainty
01-a
1.61
-
-
124
-
-
-
-
-
T
01-b
1.61
-
-
124
-
-
-
-
-
T
02
-
-
-
67.16
1.46
3.64
-
-
-
E
03
-
-
-
135
-
-
-
-
-
E
04
-
-
-
136.59
-
-
-
-
-
E
05
-
-
-
-
-
-
-
-
-
-
06
-
-
-
-
-
-
-
-
-
-
07
-
-
-
136.5
-
-
81.2
-
-
E
08
-
-
-
-
-
-
-
-
-
-
09
-
-
-
88.91
-
-
70.2
-
-
E
10
3.11
-
0.12
96
-
4.05
47.8
-
-
T
11
