Results from UNEP 2 nd Interlaboratory
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1 Results from UNEP 2 nd Interlaboratory Overview on the intercalibration data of dl-pops Van Bavel B 1, Van der Veen I 2, Nilsson H 1, De Boer J 2, Fiedler H 3 1 Örebro University, School of Science and Technology, MTM Research Center, SE Örebro, Sweden 2 VU University, Institute for Environmental Studies (IVM), De Boelelaan 1087, NL 1081 HV Amsterdam, The Netherlands 3 UNEP Chemicals Branch, chemin des Anemones, CH 1219 Châtelaine (GE), Switzerland
2 MTM Research Center School of Science & Technology Örebro University Sweden
3 Without Örebro, no Nobel price!
4 Objectives UNEP To be able to confirm a 50% decline in the levels of POPs within a 10 year period Analytical variance of the data < 25% 2 x RSD of 12.5% Z scores = 2, corresponds to 25%
5 Present State of the Art dl-pops years of QA/QC studies for dioxins From 1992 to 2011 the 16 th round More than 200 laboratories registered Participation of around 100 every year More than data points Summarized in feature article Anal. Chem. 1 1 Long-Term Wordwide QA/QC of Dioxins and Dioxin-like PCBs in Environmental Samples. Anal. Chem. 80 (2008)
6 State of the art dl-pops 2010 RSD vs. Matrix RSD (%) Incineration Soil/Sediment/Sludge Extracts Standards Incineration Soil/Sediment/Sludge Extracts Standards Fly Ash < 20% RSD Soil/Sediment < 15% RSD Standard solution < 10% *Based on 1998 WHO TEQ
7 2 nd UNEP Interlaboratory Assessment Matrices Standard solution Human milk Human blood Air Fish Sediment Water Transformer oil All laboratories were asked to re check data after reporting.
8 Traceability Sample Shipment Special metal container Adsorbent for organic solvents Cooling for milk/blood Samples send by international carrier DHL Shipment can be traced on the www Problems Clearance problems Clearance problems solved by carrier Number of Shipments > 100 shipment in Asia, South America and Africa
9 Chemical Analysis of dl-pops Use own method Standard method In house methods UNEP training Use own standard solution for calibration Or UNEP standards from training Internal QA/QC Check laboratory blanks QA/QC or SRM sample QA/QC charts
10 Report form dl-pops
11 Additional Information
12 UNEP Recommendations Implementation Recovery % (Report recovery) S/N (Report LOD, LOQ, MDL) Less than value for UB or LB Difference upper bound lower bound Report both UB and LB Individual congeners and TEQ PCB TEQ All congeners
13 Consensus value Outliers/Extreme removal traditional Data does not follow a normal Gaussian distribution Z-scores depending real RSD of the data Cofino statistic Tolerates also non Gaussian distribution Successfully used in Quasimeme and other studies Often similar to average or median
14 Cofino statistics1 1. W.P. Cofino, I.H.M. van Stokkum, J. van Steenwijk, D.E. Wells, Anal. Chim. Acta 533 (2005) 31.
15 Advanced Statistics Cofino Statistics Best fit to model Assigned value based on consensus values for all data Treatment non normal distributed data Z scores Z score= Based on set RSD of 12.5% (z = 2, 25%)
16 The Horowitz equation Dioxin Thompson Horwitz application range 1E-15 1E-14 1E-13 1E-12 1E-11 1E-10 1E-09 1E-08 1E-07 1E-06 1E-05 1E-04 0,001 0,01 0,1 1 (%) RSD Reproducibility Concentration of analyte * Eppe et al. Chemsphere 2009
17 Global distribution of the laboratories participating in the 2 nd UNEP Interlaboratory Assessment 2012/2013 N=105 laboratories, 90 reported data
18 Participation per compound class Group Standard solutions Sediment Fish Mothers milk Air Water Human serum Transformer oil OCP PCB dl-pops PBDE PFAS
19 Standard solution
20 PCDD/DF TEQ Standard solution
21 dl-pcbs TEQ standard solution
22 Summary Standard Solution dl-pops Standard solution Analyte n AV Median Mean Min Max Between lab CV (%) Inclusion rate (%) 2,3,7,8-TeCDD ,2,3,7,8-PnCDD ,2,3,4,7,8-HxCDD ,2,3,6,7,8-HxCDD ,2,3,7,8,9-HxCDD ,2,3,4,6,7,8-HpCDD OCDD ,3,7,8-TeCDF ,2,3,7,8-PnCDF ,3,4,7,8-PnCDF ,2,3,4,7,8-HxCDF ,2,3,6,7,8-HxCDF ,2,3,7,8,9-HxCDF ,3,4,6,7,8-HxCDF ,2,3,4,6,7,8-HpCDF ,2,3,4,7,8,9-HpCDF OCDF WHO1998-TEQ (PCDD PCDF) LB (ND = 0) WHO1998-TEQ (PCDD PCDF) UB (ND = LOD) PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB WHO1998-TEQ (dl-pcb) LB (ND = 0) WHO1998-TEQ (dl-pcb) UB (ND = LOD) WHO1998-TEQ (total) LB (ND = 0) WHO1998-TEQ (total) UB (ND = LOD)
23 Percentage satisfactory data n = 48 Standard Solution dl-pops 2,3,7,8-TeCDD 1,2,3,7,8-PnCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 1,2,3,4,6,7,8-HpCDD OCDD 2,3,7,8-TeCDF 1,2,3,7,8-PnCDF 2,3,4,7,8-PnCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,4,6,7,8-HpCDF 1,2,3,4,7,8,9-HpCDF OCDF TEQ (PCDD PCDF) LB TEQ (PCDD PCDF) UB PCB 77 PCB 81 PCB 126 PCB 169 PCB 105 PCB 114 PCB 118 PCB 123 PCB 156 PCB 157 PCB 167 PCB 189 TEQ (dl-pcb) LB TEQ (dl-pcb) UB TEQ (total) LB TEQ (total) UB
24 Summary Sediment dl-pops n = 34 Sediment Analyte n AV Median Mean Min Max Between lab CV (%) Inclusion rate (%) 2,3,7,8-TeCDD ,2,3,7,8-PnCDD ,2,3,4,7,8-HxCDD ,2,3,6,7,8-HxCDD ,2,3,7,8,9-HxCDD ,2,3,4,6,7,8-HpCDD OCDD ,3,7,8-TeCDF ,2,3,7,8-PnCDF ,3,4,7,8-PnCDF ,2,3,4,7,8-HxCDF ,2,3,6,7,8-HxCDF ,2,3,7,8,9-HxCDF 32 NA ,3,4,6,7,8-HxCDF ,2,3,4,6,7,8-HpCDF ,2,3,4,7,8,9-HpCDF OCDF WHO1998-TEQ (PCDD PCDF) LB (ND = 0) WHO1998-TEQ (PCDD PCDF) UB (ND = LOD) PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB WHO1998-TEQ (dl-pcb) LB (ND = 0) WHO1998-TEQ (dl-pcb) UB (ND = LOD) WHO1998-TEQ (total) LB (ND = 0) WHO1998-TEQ (total) UB (ND = LOD)
25 2,3,7,8-TeCDD 1,2,3,7,8-PnCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 1,2,3,4,6,7,8-HpCDD OCDD 2,3,7,8-TeCDF 1,2,3,7,8-PnCDF 2,3,4,7,8-PnCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,4,6,7,8-HpCDF 1,2,3,4,7,8,9-HpCDF OCDF TEQ (PCDD PCDF) LB TEQ (PCDD PCDF) UB PCB 77 PCB 81 PCB 126 PCB 169 PCB 105 PCB 114 PCB 118 PCB 123 PCB 156 PCB 157 PCB 167 PCB 189 TEQ (dl-pcb) LB TEQ (dl-pcb) UB TEQ (total) LB TEQ (total) UB NA Percentage satisfactory data n = 34 Sediment dl-pops
26 Summary Fish dl-pops n = 41 Fish Analyte n AV Median Mean Min Max Between lab CV (%) Inclusion rate (%) 2,3,7,8-TeCDD 32 NA ,2,3,7,8-PnCDD 26 NA ,2,3,4,7,8-HxCDD 16 NA ,2,3,6,7,8-HxCDD 22 NA ,2,3,7,8,9-HxCDD 18 NA ,2,3,4,6,7,8-HpCDD 26 NA OCDD 31 NA ,3,7,8-TeCDF 36 NA ,2,3,7,8-PnCDF 34 NA ,3,4,7,8-PnCDF 33 NA ,2,3,4,7,8-HxCDF 31 NA ,2,3,6,7,8-HxCDF 27 NA ,2,3,7,8,9-HxCDF 15 NA ,3,4,6,7,8-HxCDF 18 NA ,2,3,4,6,7,8-HpCDF 23 NA ,2,3,4,7,8,9-HpCDF 18 NA OCDF 22 NA WHO1998-TEQ (PCDD PCDF) LB (ND = 0) 38 NA WHO1998-TEQ (PCDD PCDF) UB (ND = LOD) 37 NA PCB PCB NA PCB NA PCB NA PCB PCB PCB PCB PCB PCB PCB PCB WHO1998-TEQ (dl-pcb) LB (ND = 0) 41 NA WHO1998-TEQ (dl-pcb) UB (ND = LOD) 40 NA WHO1998-TEQ (total) LB (ND = 0) 39 NA WHO1998-TEQ (total) UB (ND = LOD) 39 NA
27 0 Percentage satisfactory data n = 41 Fish dl-pops 2,3,7,8-TeCDD 1,2,3,7,8-PnCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 1,2,3,4,6,7,8-HpCDD OCDD 2,3,7,8-TeCDF 1,2,3,7,8-PnCDF 2,3,4,7,8-PnCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,4,6,7,8-HpCDF 1,2,3,4,7,8,9-HpCDF OCDF TEQ (PCDD PCDF) LB TEQ (PCDD PCDF) UB PCB 77 PCB 81 PCB 126 PCB 169 PCB 105 PCB 114 PCB 118 PCB 123 PCB 156 PCB 157 PCB 167 PCB 189 TEQ (dl-pcb) LB TEQ (dl-pcb) UB TEQ (total) LB TEQ (total) UB
28 Summary Mothers Milk dl-pops n = 29 Mothers milk Analyte n AV Median Mean Min Max Between lab CV (%) Inclusion rate (%) 2,3,7,8-TeCDD 18 NA ,2,3,7,8-PnCDD ,2,3,4,7,8-HxCDD 19 NA ,2,3,6,7,8-HxCDD ,2,3,7,8,9-HxCDD ,2,3,4,6,7,8-HpCDD OCDD ,3,7,8-TeCDF ,2,3,7,8-PnCDF 19 NA ,3,4,7,8-PnCDF ,2,3,4,7,8-HxCDF ,2,3,6,7,8-HxCDF ,2,3,7,8,9-HxCDF ,3,4,6,7,8-HxCDF ,2,3,4,6,7,8-HpCDF ,2,3,4,7,8,9-HpCDF 16 NA OCDF WHO1998-TEQ (PCDD PCDF) LB (ND = 0) WHO1998-TEQ (PCDD PCDF) UB (ND = LOD) PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB WHO1998-TEQ (dl-pcb) LB (ND = 0) WHO1998-TEQ (dl-pcb) UB (ND = LOD) WHO1998-TEQ (total) LB (ND = 0) WHO1998-TEQ (total) UB (ND = LOD)
29 Percentage satisfactory data n = 29 Mothers Milk dl-pops 2,3,7,8-TeCDD 1,2,3,7,8-PnCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 1,2,3,4,6,7,8-HpCDD OCDD 2,3,7,8-TeCDF 1,2,3,7,8-PnCDF 2,3,4,7,8-PnCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,4,6,7,8-HpCDF 1,2,3,4,7,8,9-HpCDF OCDF TEQ (PCDD PCDF) LB TEQ (PCDD PCDF) UB PCB 77 PCB 81 PCB 126 PCB 169 PCB 105 PCB 114 PCB 118 PCB 123 PCB 156 PCB 157 PCB 167 PCB 189 TEQ (dl-pcb) LB TEQ (dl-pcb) UB TEQ (total) LB TEQ (total) UB NA NA NA
30 PCDD/DF in Air Extract
31 Dl-PCB TEQ Air Extract
32 Air extract Analyte Summary Air Extract dl-pops n = 37 Between lab Inclusion n AV Median Mean Min Max CV (%) rate (%) 2,3,7,8-TeCDD ,2,3,7,8-PnCDD ,2,3,4,7,8-HxCDD ,2,3,6,7,8-HxCDD ,2,3,7,8,9-HxCDD ,2,3,4,6,7,8-HpCDD OCDD ,3,7,8-TeCDF ,2,3,7,8-PnCDF ,3,4,7,8-PnCDF ,2,3,4,7,8-HxCDF ,2,3,6,7,8-HxCDF ,2,3,7,8,9-HxCDF ,3,4,6,7,8-HxCDF ,2,3,4,6,7,8-HpCDF ,2,3,4,7,8,9-HpCDF OCDF WHO1998-TEQ (PCDD PCDF) LB (ND = 0) WHO1998-TEQ (PCDD PCDF) UB (ND = LOD) PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB PCB WHO1998-TEQ (dl-pcb) LB (ND = 0) WHO1998-TEQ (dl-pcb) UB (ND = LOD) WHO1998-TEQ (total) LB (ND = 0) WHO1998-TEQ (total) UB (ND = LOD)
33 Percentage satisfactory data n = 37 Air Extract 2,3,7,8-TeCDD 1,2,3,7,8-PnCDD 1,2,3,4,7,8-HxCDD 1,2,3,6,7,8-HxCDD 1,2,3,7,8,9-HxCDD 1,2,3,4,6,7,8-HpCDD OCDD 2,3,7,8-TeCDF 1,2,3,7,8-PnCDF 2,3,4,7,8-PnCDF 1,2,3,4,7,8-HxCDF 1,2,3,6,7,8-HxCDF 1,2,3,7,8,9-HxCDF 2,3,4,6,7,8-HxCDF 1,2,3,4,6,7,8-HpCDF 1,2,3,4,7,8,9-HpCDF OCDF TEQ (PCDD PCDF) LB TEQ (PCDD PCDF) UB PCB 77 PCB 81 PCB 126 PCB 169 PCB 105 PCB 114 PCB 118 PCB 123 PCB 156 PCB 157 PCB 167 PCB 189 TEQ (dl-pcb) LB TEQ (dl-pcb) UB TEQ (total) LB TEQ (total) UB NA
34 Number of reporting laboratories for PCDD/PCDF per region PCDD/PCDF Standard Air Region Total solution Sediment Fish Mothers' milk extract ASIA WEOG GRULAC AFRICA CEE Total
35 Comparison 1 st and 2 nd UNEP Interlaboratory Assessment 50% PCDD/DF TEQ CV % 45% 40% 35% 30% 25% 20% 15% 10% 5% 2010/ /2013 0% Standard Air Sediment Fish Milk
36 Comparison 1 st and 2 nd UNEP Interlaboratory Assessment 50% dl PCBs CV % 45% 40% 35% 30% 25% 20% 15% 10% 5% 2010/ /2013 0% Standard Air Sediment Fish Milk
37 Conclusions dl POPs Results 2 nd UNEP Interlaboratory Assessment Overall results good In agreement with other assessment Air test sample generated very good results for PCDD/PCDF and dl PCBs (RSD < 20%) Regional capacity Unevenly distributed WEOG Asia (Japan, Korea, China) Areas for improvement More experience needed, especially for fish matrices Need for frequent participation in interlaboratory assessments
38 Results from UNEP 2 nd Interlaboratory Overview on the intercalibration data of PFOS Van Bavel B 1, Van der Veen I 2, Nilsson H 1, De Boer J 2, Fiedler H 3 1 Örebro University, School of Science and Technology, MTM Research Center, SE Örebro, Sweden 2 VU University, Institute for Environmental Studies (IVM), De Boelelaan 1087, NL 1081 HV Amsterdam, The Netherlands 3 UNEP Chemicals Branch, chemin des Anemones, CH 1219 Châtelaine (GE), Switzerland
39 Results Milk rd Fluoros Intercalibration 2010 Standard MX4 (ng/ml) After removal of abvious outliers PFCA Average Median Min Max SD %RSD n PFBA % 11 PFPeA % 11 PFHxA % 15 PFHpA % 15 PFOA % 20 PFNA % 19 PFDA % 19 PFUdA % 13 PFDoA % 14 PFTrDA % 9 PFTeDA % 10 PFHxDA NA NA 1 PFODA % 2 PFAS Average Median Min Max SD %RSD n Linear-PFBS** % 16 Linear-PFHxS** % 19 Linear-PFHpS** % 8 Linear-PFOS** % 20 Linear-PFDS** % 12 Other PFCs optional PFOSA % 3
40 Results PFOS Serum A (RSD 12%) Serum A PFOS (n = 14, RSD = 12%) 8 7 (ng/ml) SD SD SD 2 SD Participating Laboratories Low level sample, triplicate
41 Results PFOS Standard (RSD 32%) Standard PFOS (n = 11, RSD = 32%) SD SD (ng/ml) SD SD Participating Laboratories Standard, triplicate
42 Report form PFAS
43 Assitional information PFAs
44 Participation per compound class Group Standard solutions Sediment Fish Mothers milk Air Water Human serum Transformer oil OCP PCB dl-pops PBDE PFAS
45 L-PFOS Standard Solution
46 L-PFOS Standard Solution Standard solution n AV Median Mean Min Max Between lab Inclusion CV (%) rate (%) Analyte L-PFOS anion FOSA PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA L-PFBS L-PFHxS L-PFHpS L-PFDS MeFOSA EtFOSA 4 NA MeFOSE 5 NA EtFOSE 5 NA
47 PFOS in Sediment Sediment Analyte n AV Median Mean Min Max Between lab CV (%) Inclusion rate (%) L-PFOS anion FOSA Sediment % of the % of z-scores % of z-scores % of z-scores % of z-scores data received z <2 3> z >2 6> z >3 z >6 Analyte Satisfactory Questionable Unsatisfactory Extreme L-PFOS anion FOSA
48 Fish Analyte n AV Median Mean Min Max Between lab CV (%) Satisfactory (%) L-PFOS anion FOSA
49 z= 2 z= -2 Mothers milk n AV Median Mean Min Max Between lab CV (%) Satisfactory (%) Analyte L-PFOS anion FOSA 0 NA NA NA NA NA NA NA
50 Human blood Satisfactory 50%
51 PFAS Human blood Human serum Analyte n AV Median Mean Min Max Between lab CV (%) Inclusion rate (%) L-PFOS anion FOSA 0 NA NA NA NA 0.00 NA NA PFBA 3 NA PFPeA 0 NA NA NA NA NA NA NA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA 5 NA L-PFBS 2 NA NA NA NA NA L-PFHxS L-PFHpS 1 NA NA NA NA NA L-PFDS 0 NA NA NA NA NA
52 Water
53 Water (extreme value removed) Water Analyte n AV Median Mean Min Max Between lab CV (%) Satisfactory L-PFOS anion FOSA 5 NA
54 PFAS in Air Air extract Analyte n AV Median Mean Min Max Between lab CV (%) Inclusion rate (%) L-PFOS anion FOSA MeFOSA 3 NA EtFOSA 3 NA MeFOSE 3 NA EtFOSE 3 NA Air extract % of the % of z-scores % of z-scores % of z-scores % of z-scores data received z <2 3> z >2 6> z >3 z >6 Analyte Satisfactory Questionable Unsatisfactory Extreme L-PFOS anion FOSA MeFOSA EtFOSA MeFOSE EtFOSE
55 Number of reporting laboratories for PFAS per region Human PFAS Standard Region Total solution Sediment Fish Mothers' serum Air milk extract Water ASIA WEOG GRULAC AFRICA CEE Total
56 Summary
57 Thank you for your attention! The work was funded by the European Union (ENRTP) and the Global Environment Facility (GEF)
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