Characterization of Two Passive Air Samplers for Per and Polyfluoroalkyl Substances
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1 Supporting Information Characterization of Two Passive Air Samplers for Per and Polyfluoroalkyl Substances Lutz Ahrens 1,2 *, Tom Harner 1, *, Mahiba Shoeib 1, Martina Koblizkova 1, Eric J. Reiner 3,4 1 Environment Canada, Air Quality Processes Research Section, Toronto, ON, Canada, M3H 5T4 2 Swedish University of Agricultural Sciences (SLU), Department of Aquatic Sciences and Assessment, SE-75 7 Uppsala, Sweden 3 Ontario Ministry of the Environment, 125 Resources Road, Toronto, ON, Canada 4 University of Toronto, Department of Chemistry, 8 St. George Street, Toronto, ON, Canada *Corresponding author: lutz.ahrens@slu.se, phone: , fax: *Corresponding author: tom.harner@ec.gc.ca, phone: , fax: This Document Contains 16 Tables, 13 Figures and 34 pages 1 P a g e
2 Table of Contents: TABLE S1 Per and Polyfluoroalkyl Substance (PFAS) Families, Acronyms and Formulas TABLE S2 Per and Polyfluoroalkyl Substance (PFAS) Analytes, Acronyms, Supplier and Purity TABLE S3 Sampling Time, Air Volume, Total Suspended Matter (TSP) and Meteorological Data using High Volume Air Sampler TABLE S4 Sampling Time, Air Volume and Meteorological Data using Low Volume Air Sampler TABLE S5 Sampling Time, Air Volume, Total Suspended Matter (TSP) and Meteorological Data using SIP Passive Air Sampler TABLE S6 Sampling Time, Air Volume, Total Suspended Matter (TSP) and Meteorological Data using PUF Passive Air Sampler TABLE S7 Target and Qualifier Ion for the GC MS Detection and Allocation of the Internal Standards (IS) and Injection Standard (InjS) TABLE S8 Precursor and Product Ions for the HPLC MS/MS Detection and Allocation of the Internal Standards (IS) and Injection Standards (InjS) TABLE S9 Field Blanks and Limit of Detection (LOD) for the HV-AAS of the Gasphase and Particle-phase TABLE S1 Field Blanks and Limit of Detection (LOD) for the LV-AAS and Passive Air Sampling using SIP-PAS and PUF-PAS TABLE S11 Method Recoveries (%) for Measuring PFASs using Active Air Samplers (i.e., HV-AAS and LV-AAS) and Passive Air Samplers (i.e., PUF-PAS and SIP-PAS) TABLE S12 Frequency of Detected for Individual PFAS in the Atmosphere for the Gasand Particle-phase using HV-AAS, LV-AAS, SIP-PAS and PUF-PAS in Toronto, Canada TABLE S13 Predicted Equilibrium Times in Days for SIP-PAS and PUF -PAS TABLE S14 Predicted Octanol-air Partition Coefficient (log K OA ) for individual PFAS at 17.7 C and Temperature Dependence using SPARC (September 211 release w s ) TABLE S15 Pearson Correlation of Individual PFASs with Ambient Temperature using HV-AAS TABLE S16 Duplicate Measurement (Mean Standard Deviation in %) for Individual PFASs in the Atmosphere using LV-AAS, SIP-PAS and PUF-PAS FIGURE S1 Different PAS chamber configurations FIGURE S2 Schematic flow diagram for the extraction of PUF/XAD-2 sandwiches, GFF, SIP and PUF samples FIGURE S3 Breakthrough for (A) HV-AAS (n = 3) and (B) LV-AAS (n = 3) collected 2 P a g e
3 from Toronto, Canada in 21. Figures showing relative recoveries of the front column and back column in percentage. Note: If no data shown, the PFAS was not detected in the sample FIGURE S4 Accumulated amount (pg) of individual PFASs in SIP-PAS FIGURE S5 Accumulated amount (pg) of individual PFASs in PUF-PAS FIGURE S6 Uptake profiles of PFSAs using PUF-PAS (in red) and SIP-PAS (in green) FIGURE S7 Correlation of log Q PSM-A and V EQ vs log K OA for A) PFSAs, PFCAs, FTOHs, FOSAs and FOSEs in SIP-PAS and B) PFSAs, FOSAs and FOSEs for SIP-PAS vs PUF-PAS. Regression lines for SIP-PAS (solid line) and for the PUF-PAS (dashed line) are included. Note: The minimum value for Q PSM-A was used for the PFASs which did not approach equilibrium in the PSM after a deployment period of 197 days FIGURE S8 Comparison of different chamber configurations for individual PFASs using SIP-PAS. FIGURE S9 Comparison of different chamber configurations for individual PFASs using PUF-PAS Figure S1. Average air concentrations using LV-AAS (gas- and particlephase), HV-AAS (gas- and particle-phase), SIP-PAS and PUF-PAS for PFASs between March 21 and April at Toronto, Canada. Note logarithmic y-axis. FIGURE S1 Average air concentrations using LV-AAS (gas- and particle-phase), HV- AAS (gas- and particle-phase), SIP-PAS and PUF-PAS for PFASs between March 21 and April at Toronto, Canada. Note logarithmic y-axis. FIGURE S11 Comparison of air concentrations (pg m 3) for PFASs derived using PUF- PAS and SIP-PAS. The dotted 1:1 line represents a perfect agreement and the two dashed lines represent a factor of two difference in either direction. FIGURE S12 Composition profile for the total air concentration (sum of gas- and particlephase) of the different PFAS classes measured by HV-AAS. FIGURE S13 Individual PFAS concentrations measured by four different sampling techniques over one year. The AAS include HV-AAS and LV-AAS (sum of gas- and particle phase), and the PAS include SIP-PAS and PUF-PAS. 3 P a g e
4 Sampling. High volume active air samples were collected using a PS-1 type sampler (Tisch Environmental, Cleves, OH, USA) (~33 m 3 over 24 h periods). The HV-AAS uses glass-fiber filters (GFFs) (Type A/E Glass, 12 mm diameter, Pall Corporation) for collecting the particle-phase followed by a PUF/XAD 2 cartridge for trapping the gasphase compounds. The PUF/XAD-2 cartridge consisted of 15 g of XAD 2 resin (Supelpak TM 2, precleaned from Supleco) sandwiched between a PUF plug (76 mm diameter and 6 mm thick, precleaned from Supelco) that was cut in half. Low volume air samples (~46 m 3, integrated over 14 days) were collected using a BGI- 4-4 personal LV-AAS (from BGI Inc., Waltham, MA, USA). The sampling rate was adjusted to ~3.3 m 3 day 1 (~2.3 L min 1 ) to be in the same range as previously estimated sampling rates of SIP-PAS. 1 The LV-AAS uses a PUF/XAD 2 cartridge for trapping the gas- and particle-phase compounds (i.e., no GFF was used in the LV-AAS). The PUF/XAD 2 consist of 1.5 g of XAD-2 sandwiched between a PUF plug (22 mm diameter and 76 mm long, precleaned from Supelco) that was cut in half and placed in the ORBO- 1 glass sampling head (Supelco, Bellefonte, PA, USA). Quality Assurance/Quality Control. Quantification of C 13, C 15, C 16 and C 18 (PFTriDA, PFPeDA, PFHxDA, PFOcDA) PFCAs was based on the MS/MS parameters of C 14 PFCA (PFTeDA), as analytical standards for these analytes were not available. Hence, the results given for these PFCAs should be considered as semi quantitative. Average recoveries were 78%, 96%, 67%, 81%, and 93% for the LV-AAS, SIP-PAS, PUF-PAS, and gas phase and particle using HV-AAS, respectively (Table S11). However, low recoveries of less than 3% were found for 6:2 FTOH (except for GFF samples using HV-AAS with an average value of 72%) and is therefore excluded from discussion. High recoveries were observed for the mass-labeled FOSEs because of signal enhancement during GC/MS determination. The recovery is corrected by their labeled counterpart spiked before extraction. Duplicate measurements showed excellent agreement and very good reproducibility for all sampling techniques with a mean standard deviation of ~5% for the PFASs (see Table S16). Storage stability tests showed that the sample media remain stable at 2 C for at least three month. Breakthrough experiments were conducted to check the efficiency of the PUF/XAD sandwich for trapping the gas-phase compounds using HV-AAS (n = 3, air 4 P a g e
5 volume ~33 m 3 ) and LV-AAS (n = 3, air volume ~46 m 3 ). For the HV-AAS, breakthrough was only observed for the FTOHs, 8:2 FTAC and MeFOSA with a relative proportion of 6 3% in the back column (Figure S3 in the SI). For the LV-AAS, the breakthrough was lower with a relative proportion of 2% and 4% for PFBS and 8:2 FTOH, respectively (for details see Figure S3). Correlation of the K PSM A with Octanol-air Partition Coefficient (K OA ). Previous studies have shown a correlation between log K PSM-A and log K OA (Shoeib and Harner, 22). The K OA values for individual PFASs were calculated using SPARC (September 211 release w s ) at 17.7 C, which was the average temperature during the deployment period (for details see Table S14 in the SI). In Figure S7, log Q PSM-A and V EQ were plotted against K OA for SIP-PAS and PUF-PAS. For the SIP-PAS, the slope of the regression line for the plot log Q PSM-A vs log K OA was statistically significant correlated (p <.5, Pearson Correlation). But, the slope value was only.1, which show that K OA is not a good predictor for the Q PSM-A for PFASs. However, most PFASs appeared to be in the curvilinear phase in the end of the uptake study, which indicates that the actual K PSM A is likely higher than listed in Tables 1 and 2. Interestingly, the comparison of the log-log plot Q PSM-A vs K OA for the SIP-PAS and PUF-PAS showing a higher sampling capacity for the SIP-PAS by approximately a half log unit. This underlines that the addition of XAD-4 powder to the PUF disks greatly increase the sorptive capacity of the SIP-PAS for PFASs. The log Q PSM-A was also plotted against the log subcooled liquid vapor pressure (p o L) for both PSM, but no significant correlation was found. Ultimately, the K OA or p o L cannot be used to estimate the equilibration time for other PFASs in SIP-PAS and PUF-PAS due to the low dependency between the log-log plots Q PSM-A vs K OA and p o L, respectively. However, other factors may have an impact on the partitioning of PFASs to the PSM and should be investigated in the future. 5 P a g e
6 Table S1. Per and Polyfluoroalkyl Substance (PFAS) Families, Acronyms and Formulas name of family acronym formula perfluoroalkane sulfonic acids PFSAs C n F 2n+1 SO 3 H perfluoroalkyl carboxylic acids PFCAs C n F 2n+1 COOH n:2 fluorotelomer alcohols n:2 FTOHs C n F 2n+1 CH 2 CH 2 OH n:2 fluorotelomer methacrylates n:2 FTMACs C n F 2n+1 CH 2 CH 2 OC(O)C(CH 3 )=CH 2 n:2 fluorotelomer acrylates n:2 FTACs C n F 2n+1 CH 2 CH 2 OC(O)CH=CH 2 perfluorooctane sulfonamides FOSAs C 8 F 17 SO 2 N(C n H 2n+1 )H perfluorooctane sulfonamidoethanols FOSEs C 8 F 17 SO 2 N(C n H 2n+1 )CH 2 CH 2 OH N,N-dimethyl perfluorooctane sulfonamides Me 2 FOSAs C 8 F 17 SO 2 N(CH 3 )(CH 3 ) 6 P a g e
7 Table S2. Per and Polyfluoroalkyl Substance (PFAS) Analytes, Acronyms, Supplier and Purity Analyte acronym supplier (purity) target analytes perfluorobutane sulfonic acid PFBS Wellington Laboratories (>98%) perfluorohexane sulfonic acid PFHxS Wellington Laboratories (>98%) perfluorooctane sulfonic acid PFOS Aldrich (98%) perfluorodecane sulfonic acid PFDS Wellington Laboratories (>98%) perfluorobutanoic acid PFBA Wellington Laboratories (>98%) perfluoropentanoic acid PFPeA Wellington Laboratories (>98%) perfluorohexanoic acid PFHxA Wellington Laboratories (>98%) perfluoroheptanoic acid PFHpA Aldrich (99%) perfluorooctanoic acid PFOA Aldrich (96%) perfluorononanoic acid PFNA Aldrich (97%) perfluorodecanoic acid PFDA Aldrich (98%) perfluoroundecanoic acid PFUnDA Aldrich (98%) perfluorododecanoic acid PFDoDA Aldrich (98%) perfluorotetradecanoic acid PFTeDA Aldrich (98%) 6:2 fluorotelomer alcohol 6:2 FTOH Wellington Laboratories (>98%) 8:2 fluorotelomer alcohol 8:2 FTOH Wellington Laboratories (>98%) 1:2 fluorotelomer alcohol 1:2 FTOH Wellington Laboratories (>98%) 6:2 fluorotelomer methacrylate 6:2 FTMAC Fluoryx, Inc. (>99%) 8:2 fluorotelomer acrylate 8:2 FTAC Fluoryx, Inc. (>99%) 1:2 fluorotelomer acrylate 1:2 FTAC Fluoryx, Inc. (>91%) perfluorooctane sulfonamide FOSA Wellington Laboratories (>98%) N-methyl perfluorooctane sulfonamide MeFOSA Wellington Laboratories (>98%) N-ethyl perfluorooctane sulfonamide EtFOSA Wellington Laboratories (>98%) N-methyl perfluorooctane sulfonamidoethanol MeFOSE Wellington Laboratories (>98%) N-ethyl perfluorooctane sulfonamidoethanol EtFOSE Wellington Laboratories (>98%) mass-labeled internal standards (IS) perfluoro-( 18 O 2 )-hexane sulfonic acid 18 O 2 -PFHxS Wellington Laboratories (>98%) perfluoro-( 13 C 4 )-octane sulfonic acid 13 C 4 -PFOS Wellington Laboratories (>98%) perfluoro-( 13 C 4 )-butanoic acid 13 C 4 -PFBA Wellington Laboratories (>98%) perfluoro-( 13 C 2 )-hexanoic acid 13 C 2 -PFHxA Wellington Laboratories (>98%) perfluoro-( 13 C 8 )-octanoic acid 13 C 8 -PFOA Wellington Laboratories (>98%) perfluoro-( 13 C 5 )-nonanoic acid 13 C 5 -PFNA Wellington Laboratories (>98%) perfluoro-( 13 C 2 )-decanoic acid 13 C 2 -PFDA Wellington Laboratories (>98%) perfluoro-( 13 C 2 )-undecanoic acid 13 C 2 -PFUnDA Wellington Laboratories (>98%) perfluoro-( 13 C 2 )-dodecanoic acid 13 C 2 -PFDoDA Wellington Laboratories (>98%) 2-perfluorohexyl-( 13 C 2 )-ethanol 13 C 2, D 2-6:2 FTOH Wellington Laboratories (>98%) 2-perfluorooctyl-( 13 C 2 )-ethanol 13 C 2, D 2-8:2 FTOH Wellington Laboratories (>98%) 2-perfluorodecyl-( 13 C 2 )-ethanol 13 C 2, D 2-1:2 FTOH Wellington Laboratories (>98%) perfluoro-1-( 13 C 8 )octane sulfonamide 13 C 8 -FOSA Wellington Laboratories (>98%) N-methyl-d 3 -perfluorooctane sulfonamide D 3 -MeFOSA Wellington Laboratories (>98%) N-ethyl-d 5 -perfluorooctane sulfonamide D 5 -EtFOSA Wellington Laboratories (>98%) N-methyl-d 7 -perfluorooctane sulfonamido ethanol D 7 -MeFOSE Wellington Laboratories (>98%) N-ethyl-d 9 -perfluorooctane sulfonamido ethanol D 9 -EtFOSE Wellington Laboratories (>98%) injection standards (InjS) and depuration compounds perfluoro-( 13 C 8 )-octane sulfonic acid 13 C 8 -PFOS Wellington Laboratories (>98%) perfluoro-( 13 C 4 )-octanoic acid 13 C 4 -PFOA Wellington Laboratories (>98%) N,N-dimethyl perfluorooctane sulfonamide Me 2 FOSA Wellington Laboratories (>98%) Perfluoroheptylethanol 7:2 sftoh Wellington Laboratories (>98%) 7 P a g e
8 Table S3. Sampling Time, Air Volume, Total Suspended Matter (TSP) and Meteorological Data using High Volume Air Sampler sample ID start time (EST) end time (EST) flow rate air volume TSP a average temperature total rain total snow total precipitation rel. humidity wind direction wind speed (dd/mm/yy) (hh:mm) (dd/mm/yy) (hh:mm) (m 3 h 1 ) (m 3 ) (µg m 3 ) ( C) (mm) (cm) (mm) (%) (1's deg) (km h 1 ) weather condition C1 3/3/21 15:2 31/3/21 14: clear-cloudy C2 31/3/21 14:52 1/4/21 14: cloudy C3 6/4/21 14:4 7/4/21 18: cloudy-rain C4 7/4/21 18:3 8/4/21 17: cloudy-rain C5 13/4/21 15:2 14/4/21 13: clear C6 14/4/21 14:17 15/4/21 14: clear-cloudy C8 2/4/21 11:15 21/4/21 1: clear-cloudy C9 21/4/21 11:55 22/4/21 11: clear-cloudy C1 27/4/21 13:2 28/4/21 12: clear C11 28/4/21 12:5 29/4/21 13: clear C12 4/5/21 13:18 5/5/21 13: cloudy-rain C13 11/5/21 13:45 12/5/21 13: rain C14 18/5/21 13:31 19/5/21 13: clear-cloudy C15 25/5/21 15: 26/5/21 15: clear C16 1/6/21 14:2 2/6/21 14: clear-cloudy C17 8/6/21 11:53 9/6/21 11: cloudy-rain C18 15/6/21 11:12 16/6/21 11: cloudy-rain C19 22/6/21 14:5 23/6/21 14: clear-cloudy C21 29/6/21 15:45 3/6/21 15: clear C22 6/7/21 15:15 7/7/21 16: clear-cloudy C23 13/7/21 1:55 14/7/21 : cloudy C24 15/7/21 17:5 16/7/21 16: cloudy-rain C25 21/7/21 12:5 22/7/21 16: clear-cloudy C26 27/7/21 12:28 28/7/21 13: clear-cloudy C27 3/8/21 13:3 4/8/21 14: clear-cloudy C28 1/8/21 14:56 11/8/21 16: clear-cloudy C29 17/8/21 13:12 18/8/21 13: cloudy C3 23/8/21 1:4 24/8/21 16: cloudy C32 31/8/21 14:45 1/9/21 15: clear C33 7/9/21 13:52 8/9/21 14: cloudy-rain C34 14/9/21 14:1 15/9/21 14: clear-cloudy C35 21/9/21 13:27 22/9/21 14: cloudy-rain C36 27/9/21 9:53 28/9/21 1: rain 8 P a g e
9 (continued) C37 5/1/21 13:34 6/1/21 14: rain C38 12/1/21 13:44 13/1/21 13: clear a TSP was determined gravimetrically by weighing the GFFs before and after sampling and dividing the mass by the air sample volumes. The GFFs were equilibrated before and after sampling for 24 h in an equilibration chamber containing a saturated sodium chloride solution. Table S4. Sampling Time, Air Volume and Meteorological Data using Low Volume Air Sampler sample ID start time end time flow rate air average total total total rel. wind wind (EST) (EST) volume temperature rain snow precipitation humidity direction speed (dd/mm/yy) (hh:mm) (dd/mm/yy) (hh:mm) (m 3 h 1 ) (m 3 ) ( C) (mm) (cm) (mm) (%) (1's deg) (km h 1 ) LowVol-21-C1 3/3/21 15:23 13/4/21 11: LowVol-21-C2 13/4/21 15:15 27/4/21 13: LowVol-21-C4 27/4/21 13:45 11/5/21 13: LowVol-21-C6 11/5/21 13:32 25/5/21 14: LowVol-21-C8 25/5/21 14:53 8/6/21 11: LowVol-21-C9 8/6/21 11:48 22/6/21 14: LowVol-21-C1 22/6/21 15:5 6/7/21 15: LowVol-21-C11 6/7/21 15:8 22/7/21 16: LowVol-21-C12 22/7/21 16:48 3/8/21 13: LowVol-21-C13 3/8/21 13:25 17/8/21 13: LowVol-21-C14 17/8/21 13:8 31/8/21 14: LowVol-21-C16 31/8/21 14:4 15/9/21 14: LowVol-21-C17 15/9/21 14:49 28/9/21 1: LowVol-21-C18 28/9/21 1:16 13/1/21 13: P a g e
10 Table S5. Sampling Time, Air Volume, Total Suspended Matter (TSP) and Meteorological Data using SIP Passive Air Sampler sample ID start time end time Sampling average total rain total snow total rel. wind wind speed (EST) (EST) days temperature precipitation humidity direction (dd/mm/yy) (dd/mm/yy) (days) ( C) (mm) (cm) (mm) (%) (1's deg) (km h 1 ) calibration # 1 SIP 3/3/21 6/4/ calibration # 2 SIP 3/3/21 13/4/ calibration # 3 SIP 3/3/21 2/4/ calibration # 4 SIP 3/3/21 27/4/ calibration # 4 SIP dupl. 3/3/21 27/4/ calibration # 5 SIP 3/3/21 11/5/ calibration # 6 SIP 3/3/21 25/5/ calibration # 7 SIP 3/3/21 22/6/ calibration # 7 SIP dupl. 3/3/21 22/6/ calibration # 8 SIP 3/3/21 2/7/ calibration # 9 SIP 3/3/21 17/8/ calibration # 1 SIP 3/3/21 14/9/ calibration # 11 SIP 3/3/21 13/1/ calibration # 11 SIP dupl. 3/3/21 13/1/ flush chamber # 1 SIP 3/3/21 27/4/ flush chamber # 2 SIP 27/4/21 25/5/ flush chamber # 3 SIP 25/5/21 22/6/ flush chamber # 4 SIP 22/6/21 2/7/ flush chamber # 5 SIP 2/7/21 17/8/ cm-gap chamber # 1 SIP 3/3/21 27/4/ cm-gap chamber # 2 SIP 27/4/21 25/5/ cm-gap chamber # 3 SIP 25/5/21 22/6/ cm-gap chamber # 4 SIP 22/6/21 2/7/ cm-gap chamber # 5 SIP 2/7/21 17/8/ cm-gap chamber # 1 SIP 3/3/21 27/4/ cm-gap chamber # 2 SIP 27/4/21 25/5/ cm-gap chamber # 3 SIP 25/5/21 22/6/ cm-gap chamber # 4 SIP 22/6/21 2/7/ cm-gap chamber # 5 SIP 2/7/21 17/8/ original chamber # 1 SIP 3/3/21 27/4/ original chamber # 2 SIP 27/4/21 25/5/ original chamber # 3 SIP 25/5/21 22/6/ original chamber # 4 SIP 22/6/21 2/7/ original chamber # 5 SIP 2/7/21 17/8/ P a g e
11 Table S6. Sampling Time, Air Volume, Total Suspended Matter (TSP) and Meteorological Data using PUF Passive Air Sampler sample ID start time end time Sampling average total rain total snow total rel. wind wind speed (EST) (EST) days temperature precipitation humidity direction (dd/mm/yy) (dd/mm/yy) (days) ( C) (mm) (cm) (mm) (%) (1's deg) (km h 1 ) calibration # 1 PUF 3/3/21 6/4/ calibration # 2 PUF 3/3/21 13/4/ calibration # 3 PUF 3/3/21 2/4/ calibration # 4 PUF 3/3/21 27/4/ calibration # 4 PUF dupl. 3/3/21 27/4/ calibration # 5 PUF 3/3/21 11/5/ calibration # 6 PUF 3/3/21 25/5/ calibration # 7 PUF 3/3/21 22/6/ calibration # 7 PUF dupl. 3/3/21 22/6/ calibration # 8 PUF 3/3/21 2/7/ calibration # 9 PUF 3/3/21 17/8/ calibration # 1 PUF 3/3/21 14/9/ calibration # 11 PUF 3/3/21 13/1/ calibration # 11 PUF dupl. 3/3/21 13/1/ flush chamber # 1 PUF 3/3/21 27/4/ flush chamber # 2 PUF 27/4/21 25/5/ flush chamber # 3 PUF 25/5/21 22/6/ flush chamber # 4 PUF 22/6/21 2/7/ flush chamber # 5 PUF 2/7/21 17/8/ cm-gap chamber # 1 PUF 3/3/21 27/4/ cm-gap chamber # 2 PUF 27/4/21 25/5/ cm-gap chamber # 3 PUF 25/5/21 22/6/ cm-gap chamber # 4 PUF 22/6/21 2/7/ cm-gap chamber # 5 PUF 2/7/21 17/8/ cm-gap chamber # 1 PUF 3/3/21 27/4/ cm-gap chamber # 2 PUF 27/4/21 25/5/ cm-gap chamber # 3 PUF 25/5/21 22/6/ cm-gap chamber # 4 PUF 22/6/21 2/7/ cm-gap chamber # 5 PUF 2/7/21 17/8/ original chamber # 1 PUF 3/3/21 27/4/ original chamber # 2 PUF 27/4/21 25/5/ original chamber # 3 PUF 25/5/21 22/6/ original chamber # 4 PUF 22/6/21 2/7/ original chamber # 5 PUF 2/7/21 17/8/ P a g e
12 Table S7. Target and Qualifier Ion for the GC MS Detection and Allocation of the Internal Standards (IS) and Injection Standard (InjS) analyte MW target ion qualifier ion (PCI) a qualifier ion (NCI) b allocation of the IS/InjS 6:2 FTOH C 2, D 2-6:2 FTOH 8:2 FTOH C 2, D 2-8:2 FTOH 1:2 FTOH C 2, D 2-1:2 FTOH 6:2 FTMAC C 2, D 2-6:2 FTOH 8:2 FTAC C 2, D 2-8:2 FTOH 1:2 FTAC C 2, D 2-1:2 FTOH MeFOSA D 3 -MeFOSA EtFOSA D 5 -EtFOSA MeFOSE D 7 -MeFOSE EtFOSE D 9 -EtFOSE 13 C 2, D 2-6:2 FTOH Me 2 FOSA 13 C 2, D 2-8:2 FTOH C 2, D 2-1:2 FTOH D 3 -MeFOSA D 5 -EtFOSA D 7 -MeFOSE D 9 -EtFOSE Me 2 FOSA a PCI, positive chemical ionization mode. b NCI, negative chemical ionization mode. 12 P a g e
13 Table S8. Precursor and Product Ions for the HPLC MS/MS Detection and Allocation of the Internal Standards (IS) and Injection Standards (InjS) analyte MW a precursor ion (Q1) (m/z) product ion 1 (Q3) (m/z) product ion 2 (Q3) (m/z) allocation of the IS/InjS PFBS O 2 -PFHxS (IS) PFHxS PFOS C 4 -PFOS (IS) PFDS PFBA C 4 -PFBA (IS) PFPeA PFHxA C 2 -PFHxA (IS) PFHpA PFOA C 8 -PFOA (IS) PFNA C 5 -PFNA (IS) PFDA C 2 -PFDA (IS) PFUnDA C 2 -PFUnDA (IS) PFDoDA C 2 -PFDoDA (IS) PFTrDA PFTeDA PFPeDA PFHxDA PFODA FOSA C 8 -FOSA (IS) 18 O 2 -PFHxS C 8 -PFOS (InjS) 13 C 4 -PFOS C 8 -FOSA C 4 -PFBA C 8 -PFOA (InjS) 13 C 2 -PFHxA C 4 -PFOA C 5 -PFNA C 2 -PFDA C 2 -PFUnDA C 2 -PFDoDA C 8 -PFOA C 8 -PFOS a MW, molecular weight. 13 P a g e
14 Table S9. Field Blanks and Limit of Detection (LOD) for the HV-AAS of the Gas-phase and Particle-phase a gas-phase (high volume air sampler) (n=6) field blanks (ng absolute) LOD (ng absolute) LODb (pg m 3 ) particle-phase (high volume GFF) (n=6) field blanks (ng absolute) LOD (ng absolute) LODb (pg m 3 ) LODc (pg µg 1 ) PFBS PFHxS PFOS PFDS nd.3.1 nd PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA nd.3.1 nd PFTeDA nd PFPeDA nd.1.2 nd PFHxDA nd.1.2 nd PFODA nd.1.2 nd :2 FTOH nd nd :2 FTOH nd :2 FTOH :2 FTMAC nd nd :2 FTAC nd nd :2 FTAC nd nd FOSA MeFOSA EtFOSA MeFOSE EtFOSE nd a nd = not detected. LOD = average of blanks + 3 standard deviation (σ). In case of the PFAS was not detected in the blank, the LOD was calculated as 3 times signal-to-noise for each compound in the lowest calibration standard. b Based on an average air volume of 32 m 3. c Based on an average total suspended particle (TSP) concentration of 35 µg m P a g e
15 Table S1. Field Blanks and Limit of Detection (LOD) for the LV-AAS and Passive Air Sampling using SIP-PAS and PUF-PAS a LV-AAS (n=3) SIP-PAS (n=6) PUF-PAS (n=6) field blanks LOD LODb (ng absolute) (ng absolute) (pg m 3 ) field blanks (ng/sip) LOD (ng/sip) LODc (pg m 3 ) field blanks (ng/puf) LOD (ng/puf) LODc (pg m 3 ) PFBS nd nd.2.18 PFHxS nd..2 nd.3.2 PFOS PFDS nd.3.5 nd PFBA PFPeA PFHxA PFHpA nd.3.3 PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFPeDA PFHxDA PFODA :2 FTOH nd nd nd :2 FTOH :2 FTOH :2 FTMAC nd nd nd :2 FTAC nd nd :2 FTAC nd nd nd FOSA nd..1 nd.1.1 MeFOSA EtFOSA MeFOSE EtFOSE a nd = not detected. LOD = average of blanks + 3 standard deviation (σ). In case of the PFAS was not detected in the blank, the LOD was calculated as 3 times signal-to-noise for each compound in the lowest calibration standard. b Based on an average air volume of 46 m 3. c Based on an average air volume of 112 m P a g e
16 Table S11. Method Recoveries (%) for Measuring PFASs using Active Air Samplers (i.e., HV- AAS and LV-AAS) and Passive Air Samplers (i.e., PUF-PAS and SIP-PAS) recovery (%) HV-AAS LV-AAS PAS PUF/XAD sandwich (gas-phase) (n=76) GFF (particle-phase) (n=76) PUF/XAD sandwich (n=23) SIP-PAS (n=42) PUF-PAS (n=42) 18 O 2 -PFHxS 78 ± ± 9 9 ± ± ± 6 13 C 4 -PFOS 65 ± 9 79 ± 7 91 ± 1 92 ± 12 9 ± C 4 -PFBA 74 ± 8 66 ± ± 9 48 ± ± 8 13 C 2 -PFHxA 7 ± ± 1 86 ± ± ± C 8 -PFOA 71 ± 8 68 ± 1 72 ± 1 75 ± 1 49 ± 3 13 C 5 -PFNA 65 ± 8 75 ± ± ± 6 38 ± C 2 -PFDA 64 ± 1 77 ± ± 15 6 ± 6 41 ± 3 13 C 2 -PFUnDA 6 ± 9 76 ± ± ± 8 5 ± C 2 -PFDoDA 58 ± 6 76 ± ± ± ± C 2, D 2-6:2 FTOH 14 ± ± 24 1 ± 5 ± 2 6 ± 2 13 C 2, D 2-8:2 FTOH 61 ± ± ± 2 5 ± 5 4 ± 3 13 C 2, D 2-1:2 FTOH 91 ± ± 3 53 ± 4 17 ± ± 8 D 3 -MeFOSA 18 ± 5 19 ± ± ± ± 11 D 5 -EtFOSA 113 ± ± 42 8 ± ± ± 12 D 7 -MeFOSE 156 ± ± ± ± ± 3 D 9 -EtFOSE 154 ± ± ± ± ± P a g e
17 Table S12. Frequency of Detection for Individual PFASs in the Atmosphere for the Gas- and Particle-phase using HV-AAS, LV-AAS, SIP-PAS and PUF-PAS in Toronto, Canada HV-AAS LV-AAS PAS gas-phase particle-phase SIP-PAS PUF-PAS PFBS 71% 7% 1% 1% 67% PFHxS 57% % 1% 1% 1% PFOS 86% 8% 88% 1% 78% PFDS % 57% % 1% 89% PFBA 87% % 41% 1% % PFPeA 87% % 12% 1% % PFHxA 79% % % 1% % PFHpA 1% % % 1% % PFOA 57% 97% 29% 85% % PFNA 69% 97% % 96% % PFDA 34% 93% % 1% % PFUnDA 29% 67% % 1% % PFDoDA % 86% % 1% % PFTrDA % 69% % 1% % PFTeDA % 61% % 1% % PFPeDA % 26% % 96% % PFHxDA % 6% % 63% % PFODA % % % 67% % 6:2 FTOH 97% 11% 71% 93% % 8:2 FTOH 1% 83% 1% 1% % 1:2 FTOH 99% 79% 1% 1% % 6:2 FTMAC 66% % 35% % % 8:2 FTAC 78% % 1% % % 1:2 FTAC 65% % 1% % % FOSA % 16% % % % MeFOSA 97% 83% 1% 1% 1% EtFOSA 93% 57% 1% 1% 1% MeFOSE 96% 99% 1% 1% 96% EtFOSE 79% 99% 1% 1% 1% Legend: % 49% 5 9% >9% 17 P a g e
18 Table S13. Predicted Equilibrium Times in Days for SIP-PAS and PUF -PAS linear phase, t 25 (days) a equilibrium phase, t 95 (days) b SIP-PAS PUF-PAS SIP-PAS PUF-PAS PFBS PFHxS PFOS PFDS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFPeDA PFHxDA PFODA 6:2 FTOH :2 FTOH :2 FTOH :2 FTMAC 8:2 FTAC 1:2 FTAC FOSA MeFOSA EtFOSA 5 52 MeFOSE EtFOSE a k U = A PSM /V PSM k A /K PSM-A and t 25 = ln(.75)/k U. b t 95 = ln(.5)/k U 18 P a g e
19 Table S14. Predicted Octanol-air Partition Coefficient (log K OA ) for individual PFAS at 17.7 o C and Temperature Dependence using SPARC (September 211 release w s ) log (K OA ) = m/(t) + b a K OA m b at 17.7 C PFBS PFHxS PFOS PFDS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFPeDA PFHxDA PFODA :2 FTOH :2 FTOH :2 FTOH :2 FTMAC :2 FTAC :2 FTAC FOSA MeFOSA EtFOSA MeFOSE EtFOSE a T in Kelvin. 19 P a g e
20 Table S15. Pearson Correlation of Individual PFASs with Ambient Temperature using HV-AAS a gas-phase particle-phase sum of gas- and particle-phase r 2 p-value r 2 p-value r 2 p-value PFBS NS PFHxS.9 NS nd -.9 NS PFOS.1 NS PFDS nd -.25 < PFBA.8.29 nd PFPeA.8.28 nd PFHxA.6 NS nd -.6 NS PFHpA nd - nd - nd - PFOA. NS.52 <.1.22 <.1 PFNA. NS.49 <.1.35 <.1 PFDA.1 NS.36 <.1.29 <.1 PFUnDA. NS.33 <.1.28 <.1 PFDoDA nd -.31 <.1.31 <.1 PFTrDA nd -.3 NS.3 NS PFTeDA nd -.3 NS.3 NS PFPeDA nd -.1 NS.1 NS PFHxDA nd -.23 NS.15 NS PFODA nd - nd - nd - 6:2 FTOH NS :2 FTOH.36 <.1.19 <.1.34 <.1 1:2 FTOH.54 <.1.5 <.1.51 <.1 6:2 FTMAC.6 NS nd -.6 NS 8:2 FTAC.24 <.1 nd :2 FTAC.24 <.1 nd -.29 <.1 FOSA nd MeFOSA.58 <.1. NS.55 <.1 EtFOSA.62 <.1.8 NS.62 <.1 MeFOSE.8 <.1.1 NS.68 <.1 EtFOSE.6 <.1.15 <.1.68 <.1 PFSAs. NS PFCAs.1 NS.58 <.1.1 NS FTOHs.37 <.1.37 <.1.36 <.1 FTMACs/FTACs.14.3 nd FOSAs.64 <.1. NS.63 <.1 FOSEs.78 <.1.1 NS.73 <.1 PFASs.39 <.1.24 <.1.4 <.1 a nd = not detected. NS = not significantly correlated. 2 P a g e
21 Table S16. Duplicate Measurement (Mean Standard Deviation in %) for Individual PFASs in the Atmosphere using LV-AAS, SIP-PAS and PUF-PAS a LV-AAS (n = 3) SIP-PAS (n = 3) PUF-PAS (n = 3) PFBS nd PFHxS nd PFOS nd PFDS nd 1.5 nd PFBA nd PFPeA nd 2.4 nd PFHxA nd 1.4 nd PFHpA nd 4. nd PFOA nd PFNA nd 1.4 nd PFDA nd.7 nd PFUnDA nd 3.8 nd PFDoDA nd 2.5 nd PFTrDA nd 3.4 nd PFTeDA nd 3. nd PFPeDA nd 11.7 nd PFHxDA nd 11.3 nd PFODA nd 6.2 nd 6:2 FTOH nd 8:2 FTOH nd 1:2 FTOH nd 6:2 FTMAC 3.6 nd nd 8:2 FTAC 5. nd nd 1:2 FTAC 5. nd nd FOSA nd nd nd MeFOSA EtFOSA MeFOSE EtFOSE a nd = not detected. 21 P a g e
22 original chamber flush chamber 1-cm gap chamber 2-cm gap chamber stainless steel dome PUF or SIP disk air circulation Figure S1. Different PAS chamber configurations. Figure S2. Schematic flow diagram for the extraction of PUF/XAD-2 sandwiches, GFF, SIP and PUF samples. 22 P a g e
23 A) HV-AAS PFBS PFHxS PFOS PFDS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFPeDA PFHxDA PFODA 6:2 FTOH 8:2 FTOH 1:2 FTOH 6:2 FTMAC 6:2 8:2 FTAC 1:2 FTAC FOSA MeFOSA EtFOSA MeFOSE EtFOSE front column back column B) LV-AAS PFBS PFHxS PFOS PFDS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFPeDA PFHxDA PFODA 6:2 FTOH 8:2 FTOH 1:2 FTOH 6:2 FTMAC 6:2 8:2 FTAC 1:2 FTAC FOSA MeFOSA EtFOSA MeFOSE EtFOSE front column back column Figure S3. Breakthrough for (A) HV-AAS (n = 3) and (B) LV-AAS (n = 3) collected from Toronto, Canada in 21. Figures showing relative recoveries of the front column and back column in percentage. Note: If no data shown, the PFAS was not detected in the sample. 23 P a g e
24 accumulated amount (pg)_ PFBA accumulated amount (pg) _ PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFPeDA PFHxDA PFODA deployment time (days) deployment time (days) 6 PFBS 3 accumulated amount (pg)_ PFHxS PFOS PFDS accumulated amount (pg)_ :2 FTOH 8:2 FTOH 1:2 FTOH deployment time (days) deployment time (days) 16 MeFOSA accumulated amount (pg)_ EtFOSA MeFOSE EtFOSE deployment time (days) Figure S4. Accumulated amount (pg) of individual PFASs in SIP-PAS. 24 P a g e
25 Figure S5. Accumulated amount (pg) of individual PFASs in PUF-PAS. Figure S6. Uptake profiles of PFSAs using PUF-PAS (in red) and SIP-PAS (in green). 25 P a g e
26 Figure S7. Correlation of log Q PSM-A and V EQ vs log K OA for A) PFSAs, PFCAs, FTOHs, FOSAs and FOSEs in SIP-PAS and B) PFSAs, FOSAs and FOSEs for SIP-PAS vs PUF-PAS. Regression lines for SIP-PAS (solid line) and for the PUF-PAS (dashed line) are included. Note: The minimum value for Q PSM-A was used for the PFASs which did not approach equilibrium in the PSM after a deployment period of 197 days. 26 P a g e
27 Figure S8. Comparison of different chamber configurations for individual PFASs using SIP- PAS. 27 P a g e
28 Figure S9. Comparison of different chamber configurations for individual PFASs using PUF- PAS. 28 P a g e
29 Figure S1. Average air concentrations using LV-AAS (gas- and particle-phase), HV-AAS (gas- and particle-phase), SIP-PAS and PUF-PAS for PFASs between March 21 and April at Toronto, Canada. Note logarithmic y-axis. Figure S11. Comparison of air concentrations (pg m 3 ) for PFASs derived using PUF-PAS and SIP-PAS. The dotted 1:1 line represents a perfect agreement and the two dashed lines represent a factor of two difference in either direction. 29 P a g e
30 Composition (%)_ 1% 8% 6% 4% 2% PFSAs PFCAs FTOHs FTMACs/FTACs FOSAs FOSEs % 3/3/21 1/6/21 31/8/21 24/11/21 11/1/211 Figure S12. Composition profile for the total air concentration (sum of gas- and particle-phase) of the different PFAS classes measured by HV-AAS. 3 P a g e
31 Concentration (pg m 3 )_ Concentration (pg m 3 )_ Concentration (pg m 3 )_ Concentration (pg m 3 )_ PFBS HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS PUF-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/ PFHxS HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS PUF-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/ PFDS HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS PUF-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/ PFBA HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/ P a g e
32 Concentration (pg m 3 )_ PFPeA HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/211 Concentration (pg m 3 )_ Concentration (pg m 3 )_ :2 FTOH HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/ :2 FTOH HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/211 Concentration (pg m 3 )_ MeFOSA HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS PUF-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/ P a g e
33 Concentration (pg m 3 )_ Concentration (pg m 3 )_ EtFOSA HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS PUF-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/ EtFOSE HV-AAS (gas- and particle-phase) LV-AAS (gas- and particle-phase) SIP-PAS PUF-PAS 3/3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/211 Concentration (pg m 3 )_ 5 4 6:2 FTMAC HV-AAS (gas- and particle-phase) /3/21 1/6/21 27/7/21 27/9/21 25/11/21 18/1/211 22/3/211 Figure S13. Individual PFAS concentrations measured by four different sampling techniques over one year. The AAS include HV-AAS and LV-AAS (sum of gas- and particle phase), and the PAS include SIP-PAS and PUF-PAS. 33 P a g e
34 REFERENCES (1) Shoeib, M.; Harner, T.; Lee, S. C.; Lane, D.; Zhu, J. Sorbent-impregnated polyurethane foam disk for passive air sampling of volatile fluorinated chemicals. Anal. Chem. 28, 8, P a g e
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