Appendix D Overview of methods applied in round 1-4 Table S3.1 Analytical techniques applied in round 1 Lab Instrument R1 Column Type volume (µL) Temperatures ( °C) Oven program3 MS Gas Flow rate4 (mL/min) Calibration & quantification method5 001 Magnetic Sector Rxi-5MS 1 90 (1min), 20/min to 245, 50/min to 300 (5min) 140 0.9 Internal, own standards: Tomy et al. [2] 003 GC-ECNI-LRMS DB-5MS 3 120 (2min), 50/min to 325 (3min) 150 1.8 External, own standards 004 GC-ECNI-LRMS Rtx-200 2 90 (1min), 120 /min to 140, 15 /min to 320 (10min) 150 1.5 Internal, linear, provided standard [a] and own standards [b] 007 GC-ToF-EI-MS 7000 DB-5MS 2 100 (5min), 20 /min to 300, (10min) 300 1.0 Internal, linear 008 GC-ECNI-LRMS 1000 2 105 (1min), 34 /min to 190 (1min), 8/min to 250, 40/min to 290 (8min) 200 0.9 Internal, Castells et al.[3], provided standard [a] own standards [b] 009 GC-ECNI-LRMS 1000 Rtx-1614 1 100 (10min), 10/min to 260 (30min) 230 NA Internal, linear forced through zero 010 GC-ECNI-LRMS 1000 DB-5MS 1 100 (1min), 15/min to 280 (10min), 10/min to 300 (10min) 150 1 Internal, Tomy et al. [2] 011 GC-EI-MS/MS Restek 10 110 (2min), 40/min to 200, 10/min to 260, 20/min to 290°C 220 1 External, linear 25
008 GC-ECNI-LRMS 1000 2 105 (1min), 34/min to 190 (1min), 8/min to 250, 40/min to 290 (8min) 200 0.9 Internal, Castells et al.[3] 009 GC-ECNI-LRMS 1000 HP5-MS 1 100 (10min), 10/min to 260 (30min) 230 NA Internal, linear 012 GC-EI-MS/MS 2 100 (2min), 50/min to 300 (2min) 250 1.5 External, linear GC-ECNI-LRMS 1000 DB-5MS 1 100 (3min), 20/min to 140, 5/min to 300 200 1.2 External, linear GC×GC-µECD NA DB1-MS Innowax 3×0.25×0.1 1 65 (2min), 20/min to 140, 3/min to 270 2706 F1 0.4 F2 30 External, linear 016 GC-ECNI-LRMS 1000 DB-5MS 2 50 (1min), 70/min to 100 (1min), 60/min to 290 (4min) 150 1.3 MLR ISO 12010 017 Magnetic Sector DB-57 2 110, 10/min to 310 120 NA, Hydrogen Internal, own standards Tomy et al. [2] 018 GC-EI-MS/MS HP-5MS 5 60 (1min), 20/min to 300 (10min) 150 1.4 Internal, linear, provided standards [a] own standards [b] 019 GC-EI-MS/MS ZB-XLBHT 2 130 (4min), 40/min to 300 230 1.4 Internal, linear 023 GC-ECNI-LRMS 1000 DB1-MS 2 110 (0.5min), 25/min to 325 (3min) 150 2.5 External R Resolving power RF Response factor NA Not available MLR Multiple linear regression 1 Approximately 2 Length m × i.d. mm × film thickness µm 3 Hold time in brackets 4 carrier gas was helium and reagent gas methane, unless otherwise stated 4 When using participants’ own standards
6 Temperature of ECD 7 Self manufactured glass column Table S3.3 Analytical techniques applied in round 3 Lab Analytical technique R1 Column Type (µL) Temperatures (°C) Oven program3 MS Gas Flow rate4 (mL/min) Calibration& Quantification method5 001 Magnetic Sector HP-1MS 1 90 (1.2min), 20/min to 245, 50/min to 300 140 1 Internal, Tomy et al. [2] 004 GC-ECNI-LRMS 1000 Rtx-200 2 90 (1min), 120/min to 140, 15/min to 320 (10min) 150 1.5 NA 008 GC-ECNI-LRMS 1000 1 105 (1min), 34/min to 190 (1min), 8/min to 250, 40/min to 290 (8min) 200 0.9 Internal, Castells et al. [3] 009 GC-ECNI-LRMS 1000 Rtx-1614 1 100 (10min), 10/min to 260 (30min) 230 NA, Helium Internal, linear GC-ECNI-LRMS 1000 DB-5MS 4 x 1 90 (2min), 15/min to 325 (10min) 200 1 External, linear 017 Magnetic Sector Rxi-5MS 2 110, 10/min to 310 120 NA, Argon Internal, Tomy et al. [2]
018 GC-EI-MS/MS HP-5MS 5 60 (1min), 20/min to 300 (5min) 280 1.4 External, quadratic 019 GC-EI-MS/MS HP-5MS 2 130 (4min), 40/min to 300 230 1.4 Internal, linear 021 GC×GC-µECD NA DB1 Rtx-PCB 1 80 (2min), 10/min to 160, 4/min to 280 (5min) 3006 1.2 External, linear 029 J&W 5 80 (1min), 50/min to 300 (4min) 120 2.6 MLR ISO 18635 030 GC-EI-MS/MS Thermo TG5-HT 1.2 25/min to 320 220 1.5, Argon External 032 CSk-GC-MS DB-5MS 1 50 (3min), 10/min to 280 (10min) 230 2, Hydrogen Internal 033 GC-ECNI-LRMS 1000 DB-5 1 60 (1min), 15/min to 320 (13.7min) 142 2 Internal, Tomy et al. [2] R Resolving power RF Response factor NA Not available MLR Multiple linear regression 1 Approximately 2 Length m × i.d. mm × film thickness µm 3 Hold time in brackets 4 carrier gas was helium and reagent gas methane, unless otherwise stated 5 When specified and when participants used their own standards 6 Temperature of ECD 18
S3.4 Analytical techniques applied in round 4 Lab Analytical technique R1 Column Type (µL) Temperatures (°C) Oven program3 MS SCCPs3 Calibration & Quantification method5 001 Magnetic Sector 8000 HP-Ultra 2 1 x 1 90 (1min), 20/min to 245, 50/min to 300 (5min) 140 C13Cl7-9 Internal, Tomy et al. [2] 008 GC-ECNI- LRMS 1000 3 x 2 105 (1min), 34/min to 190 (1min), 8/min to 250, 40/min to 290 (8min) 200 [Cl2]- and [HCl2]- ions Internal, Castells et al. [3] GC-ECNI- LRMS 1000 DB-1 4 x 1 90 (2min), 30/min to 290, 15/min to 325 (7min) 200 Internal, Reth et al. [4] GC×GC-µECD NA HP-5MS ZB-50 1 x 1 90 (2min), 10/min to 180 (2min), 1.5/min to 280, 30/min to 320 (10min) 3006 Internal, Reth et al. [4] specific
016 GC-ECNI- LRMS 1000 DB-5MS 1 x 2 80 (2min), 70/min to 280 (2min), 70/min to 300 (2min) 150 4 ions MLR ISO 18635 023 GC-ECNI- LRMS 1000 DB-1MS 1 x 2 110 (1min), 15/min to 330 150 C12Cl5-9 C13Cl5-9 External, 31 8200 None NA 1 x 5 NA NA C9Cl6-9 Internal, Bogdal et al. [5] 035 7500 HP-5MS 1 x 5 90 (1min), 25/min to 290 (3min) 150 C9Cl7-9 External, Reth et al. [4] None NA 1 x 5 NA NA Internal, Bogdal et al. [5]