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  5. Analysis for PFAS (PFOS, PFOA, PFHxS, etc.)

Analysis for PFAS (PFOS, PFOA, PFHxS, etc.)

Perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA), which are polyfluoroalkyl substances (PFCs / PFAS), are difficult to decompose in the environment and have a high accumulation potential. They are subject to various international regulations, including the Stockholm Convention on Persistent Organic Pollutants (POPs)*.

Fujifilm Wako provides pretreatment columns, solvents, and analytical standards that can be used to analyze PFAS (PFOS, PFOA, and PFHxS).

  • 00353_img01.png

    PFOS (PerFluoroOctaneSulfonic acid)
  • 00353_img02.png

    PFOA (PerFluoroOctanoic acid)
  • 00353_img08.png

    PFHxS (PerFluoroHexaneSulfonic acid)

* POPs
Chemical substances that are highly toxic, persistent, bioaccumulative, mobile over long distances, and have adverse effects on human health or the environment are called Persistent Organic Pollutants (POPs). POPs are required to eliminate / limit, reduce emissions, and properly dispose of waste.

3 PFAS Mixture Standard Solution

Fujifilm Wako provides mixture standard solutions and internal standard solution (13C labels) for PFHxS, PFOS, and PFOA which are compounds subject to JP Water Quality Act. Both are mixture standard solutions with clear concentration value of linear PFAS.

Features

✔ Mixture standard solutions with clear concentration value of linear PFAS!

LC/MS Chromatogram (3 PFCs Mixture Standard Solution)

00353_img10.png
Peak No. Constituent Monitoring Ion (m/z) Mode
1 PFOA 413 -
2 PFHxS 399 -
3 PFOS 499 -

Analysis conditions

[HPLC]
Column
： Wakopak® Ultra C18-2　2.1×100 mm
Delay column
： Wakopak® Ultra C18-3　2.0×150 mm
Column temperature
： 40 ℃
Eluent
： A) 0.01 mol/L CH3COONH4 in H2O
： B) CH3CN
Gradient
：
Time (min) B conc. (%)
0-2 20
2-22 20-95
22-30 95
Flow rate
： 0.2 mL/min.
[MS]
Ionization
： ESI
Mode
： SIM

26 PFAS Mixture Standard Solution

Features

✔ Mixture standard solutions with clear concentration value of linear PFAS!

Peak No. Name Abbreviation Monitoring Ion
(m/z)		 Mode Concentration
(μg/L)
1 Perfluorobutanoic Acid PFBA 213 - 2
2 Perfluoro-3-methoxypropanoic Acid PFMPA 229 - 2
3 Perfluoropentanoic Acid PFPeA 263 - 2
4 Perfluoro-4-methoxybutanoic Acid PFMBA 279 - 2
5 1H,1H,2H,2H-Perfluorohexanesulfonic Acid 4:2 FTS 327 - 2
6 Perfluorohexanoic Acid PFHxA 313 - 2
7 Perfluorobutanesulfonic Acid PFBS 299 - 2
8 Perfluoro(2-methyl-3-oxahexanoic) Acid GenX
(HEPO-DA)		 285 - 2
9 Perfluoro(2-ethoxyethane)sulfonic Acid PFEESA 315 - 2
10 Perfluoroheptanoic Acid PFHpA 363 - 2
11 Perfluoropentanesulfonic Acid PFPeS 349 - 2
12 1H,1H,2H,2H-Perfluorooctanesulfonic Acid 6:2 FTS 427 - 2
13 (Z)-2H-Perfluoro-2-decenoic Acid 8:2 FTUCA 457 - 2
14 Perfluorononanoic Acid PFNA 463 - 2
15 1H,1H,2H,2H-Perfluorodecanesulfonic Acid 8:2 FTS 527 - 2
16 Perfluoroheptanesulfonic Acid PFHpS 449 - 2
17 Perfluorodecanoic Acid PFDA 513 - 2
18 N-Ethylperfluoro-1-octanesulfonamidoacetic Acid N-EtFOSAA 584 - 2
19 Perfluoroundecanoic Acid PFUnDA 563 - 2
20 Perfluorododecanoic Acid PFDoDA 613 - 2
21 Perfluorooctanesulfonamide PFOSA 498 - 2
22 Perfluorodecanesulfonic Acid PFDS 599 - 2
23 Perfluorotridecanoic Acid PFTrDA 663 - 2
24 Perfluorotetradecanoic Acid PFTeDA 713 - 2
25 N-Methylperfluoro-1-octanesulfonamide N-MeFOSA 512 - 2
26 Perfluorohexadecanoic Acid PFHxDA 813 - 2

Analysis conditions

[HPLC]
Column
： Wakopak® Ultra C18-2 2.1×100 mm
Delay column
： Wakopak® Ultra C18-3 2.0×150 mm
Column temperature
： 40 ℃
Eluent
： A) 0.01 mol/L CH3COONH4 in H2O
： B) CH3CN
Gradient
：
Time (min) B conc. (%)
0-2 20
2-22 20-95
22-30 95
30-40 20
Flow rate
： 0.2 mL/min.
[MS]
Ionization
： ESI
Mode
： SIM

* Analysis conditions, chromatograms, and detected ions are reference data and do not constitute guaranteed values for this product.

3 PFAS Internal Standards Mixture Solution

Features

✔ 13C-labeled mixed internal standard solution

Peak No. Name Abbreviation Monitoring Ion
(m/z)		 Mode Concentration
(μg/L)
1 Perfluorooctanoic Acid-13C8 PFOA-13C8 421 - 2
2 Perfluorohexanesulfonic Acid-13C6 PFHxS-13C6 305 - 2
3 Perfluorooctanesulfonic Acid-13C8 PFOS-13C8 507 - 2

Analysis conditions

[HPLC]
Column
： Wakopak® Ultra C18-2 2.1×100 mm
Delay column
： Wakopak® Ultra C18-3 2.0×150 mm
Column temperature
： 40 ℃
Eluent
： A) 0.01 mol/L CH3COONH4 in H2O
： B) CH3CN
Gradient
：
Time (min) B conc. (%)
0-2 20
2-22 20-95
22-30 95
30-40 20
Flow rate
： 0.2 mL/min.
[MS]
Ionization
： ESI
Mode
： SIM

* Analysis conditions, chromatograms, and detected ions are reference data and do not constitute guaranteed values for this product.

7 PFAS Internal Standards Mixture Solution

Features

✔ 13C-labeled mixed internal standard solution

Peak No. Name Abbreviation Monitoring Ion
(m/z)		 Mode Concentration
(μg/L)
1 Perfluorobutanoic Acid-13C4 PFBA-13C4 217 - 2
2 Perfluoropentanoic Acid-13C5 PFPeA-13C5 268 - 2
3 Perfluorohexanoic Acid-13C6 PFHxA-13C6 319 - 2
4 Perfluorobutanesulfonic Acid-13C4 PFBS-13C4 303 - 2
5 Perfluoro(2-methyl-3-oxahexanoic) Acid-13C3 GenX-13C3 288 - 2
6 Perfluoroheptanoic Acid-13C7 PFHpA-13C7 370 - 2
7 Perfluorononanoic Acid-13C6 PFNA-13C6 469 - 2

Analysis conditions

[HPLC]
Column
： Wakopak® Ultra C18-2 2.1×100 mm
Delay column
： Wakopak® Ultra C18-3 2.0×150 mm
Column temperature
： 40 ℃
Eluent
： A) 0.01 mol/L CH3COONH4 in H2O
： B) CH3CN
Gradient
：
Time (min) B conc. (%)
0-2 20
2-22 20-95
22-30 95
30-40 20
Flow rate
： 0.2 mL/min.
[MS]
Ionization
： ESI
Mode
： SIM

* Analysis conditions, chromatograms, and detected ions are reference data and do not constitute guaranteed values for this product.

Analysis example

LC/MS/MS Chromatogram (3 PFCs Mixture Standard Solution＋ 26 PFCs Mixture Standard Solution)

Peak No. Name Abbreviation Monitoring Ion
(m/z)		 Mode
Precursor Product
1 Perfluorobutanoic Acid PFBA 212.95 169.00 -
2 Perfluoro-3-methoxypropanoic Acid PFMPA 229.00 85.00 -
3 Perfluoropentanoic Acid PFPeA 262.95 219.10 -
4 Perfluoro-4-methoxybutanoic Acid PFMBA 278.95 85.05 -
5 1H,1H,2H,2H-Perfluorohexanesulfonic Acid 4:2 FTS 326.95 306.90 -
6 Perfluorohexanoic Acid PFHxA 313.00 268.95 -
7 Perfluorobutanesulfonic Acid PFBS 298.95 80.00 -
8 Perfluoro(2-methyl-3-oxahexanoic) Acid GenX
(HEPO-DA)		 284.90 169.05 -
9 Perfluoro(2-ethoxyethane)sulfonic Acid PFEESA 314.95 135.00 -
10 Perfluoroheptanoic Acid PFHpA 363.00 319.00 -
11 Perfluoropentanesulfonic Acid PFPeS 349.00 80.05 -
12 1H,1H,2H,2H-Perfluorooctanesulfonic Acid 6:2 FTS 427.00 407.05 -
13 Perfluorooctanoic Acid PFOA 413.00 168.95 -
14 (Z)-2H-Perfluoro-2-decenoic Acid 8:2 FTUCA 457.00 392.95 -
15 Perfluorohexanesulfonic Acid PFHxS 398.95 80.00 -
16 Perfluorononanoic Acid PFNA 463.00 419.00 -
17 1H,1H,2H,2H-Perfluorodecanesulfonic Acid 8:2 FTS 527.00 506.85 -
18 Perfluoroheptanesulfonic Acid PFHpS 449.00 80.10 -
19 Perfluorodecanoic Acid PFDA 512.95 469.00 -
20 N-Ethylperfluoro-1-octanesulfonamidoacetic Acid N-EtFOSAA 584.00 418.90 -
21 Perfluorooctanesulfonic Acid PFOS 499.00 80.15 -
22 Perfluoroundecanoic Acid PFUnDA 563.00 518.90 -
23 Perfluorododecanoic Acid PFDoDA 612.95 569.00 -
24 Perfluorooctanesulfonamide PFOSA 498.00 77.95 -
25 Perfluorodecanesulfonic Acid PFDS 598.95 99.10 -
26 Perfluorotridecanoic Acid PFTrDA 662.95 618.95 -
27 Perfluorotetradecanoic Acid PFTeDA 712.95 668.80 -
28 N-Methylperfluoro-1-octanesulfonamide N-MeFOSA 511.95 169.05 -
29 Perfluorohexadecanoic Acid PFHxDA 812.95 768.85 -

Analysis conditions

[HPLC]
Column
： Wakopak® Ultra C18-2 2.1×100 mm
Delay column
： Wakopak® Ultra C18-3 2.0×150 mm
Column temperature
： 40 ℃
Eluent
： A) 0.01 mol/L CH3COONH4 in H2O
： B) CH3CN
Gradient
：
Time (min) B conc. (%)
0-2 20
2-22 20-95
22-30 95
30-40 20
Flow rate
： 0.2 mL/min.
[MS]
Ionization
： ESI
Mode
： SIM

* Analysis conditions, chromatograms, and detected ions are reference data and do not constitute guaranteed values for this product.

Single Analytical Standards

Structural Formula Name CAS Abbreviation Carbon Length Code No. Volume
Perfluorobutanoic Acid 375-22-4 PFBA 4 161-29301 100 mg
Perfluorobutanesulfonic Acid 375-73-5 PFBS 4 165-29821 1 mL×5A
Perfluoropentanoic Acid 2706-90-3 PFPeA 5 163-29361 100 mg
Perfluoropentanesulfonic Acid Hydrate 2828827-14-9 PFPeS 5 168-29431 50 mg
Perfluorohexanoic Acid 307-24-4 PFHxA 6 168-29311 100 mg
Perfluorohexanesulfonic Acid Potassium Salt 355-46-4
3871-99-6
(Potassium Salt)		 PFHxS 6 168-28951 100 mg
1H,1H,2H,2H-Perfluorohexanesulfonic Acid 757124-72-4 4:2 FTS 6 169-29601 100 mg
Perfluoroheptanoic Acid 375-85-9 PFHpA 7 160-29371 100 mg
Perfluoroheptanesulfonic Acid 375-92-8 PFHpS 7 165-29441 50 mg
1H,1H,2H,2H-Perfluorooctanesulfonic Acid 27619-97-2 6:2 FTS 8 166-29611 100 mg
Perfluorooctanesulfonamide 754-91-6 PFOSA 8 164-29531 100 mg
N-Methylperfluoro-1-octanesulfonamide 31506-32-8 N-MeFOSA 8 138-19521 50 mg
N-Ethylperfluoro-1-octanesulfonamidoacetic Acid 2991-50-6 N-EtFOSAA 8 051-09631 50 mg
Perfluorononanoic Acid 375-95-1 PFNA 9 165-29321 100 mg
Perfluorodecanoic Acid 335-76-2 PFDA 10 167-29381 100 mg
Perfluorodecanesulfonic Acid 335-77-3 PFDS 10 162-29451 50 mg
1H,1H,2H,2H-Perfluorodecanesulfonic Acid 39108-34-4 8:2 FTS 10 164-29391 100 mg
(Z)-2H-Perfluoro-2-decenoic Acid 161094-76-4 8:2 FTUCA 10 161-29661 50 mg
Perfluoroundecanoic Acid 2058-94-8 PFUnDA 11 162-29331 100 mg
Perfluorododecanoic Acid 307-55-1 PFDoDA 12 169-29341 100 mg
Perfluorotridecanoic Acid 72629-94-8 PFTrDA 13 165-29561 100 mg
Perfluorotetradecanoic Acid 376-06-7 PFTeDA 14 166-29351 100 mg
Perfluorohexadecanoic Acid 67905-19-5 PFHxDA 16 168-29551 100 mg
Perfluorooctadecanoic Acid 16517-11-6 PFODA 18 169-29581 100 mg
Nonafluoro-3,6-dioxaheptanoic Acid 151772-58-6 NFDHA - 148-10161 100 mg
Perfluoro-4-methoxybutanoic Acid 863090-89-5 PFMBA - 161-29421 100 mg
Perfluoro-3-methoxypropanoic Acid 377-73-1 PFMPA - 163-29621 100 mg
Perfluoro(2-ethoxyethane)sulfonic Acid 113507-82-7 PFEESA - 162-29831 1 mL×5A
Perfluoro(2-methyl-3-oxahexanoic) Acid 13252-13-6 GenX - 166-29591 100 mg

Solvents for PFAS Analysis

Features

  • Guarantees PFOA, PFOS, and PFHxS in the solvent is 1 ng/L or less.
  • Suitable for pretreatment and instrument cleaning.
  • Guarantees HPLC specification items.

Example Test Items (Methanol)

REQUIREMENT SPECIFICATION
Appearance Colorless clear liquid
Density (20 ℃) 0.789-0.792 g/mL
Refractive index n D20 1.327-1.330
Absorbance (210 nm) max.0.60
Absorbance (220 nm) max.0.30
Absorbance (230 nm) max.0.15
Absorbance (240 nm) max.0.06
Absorbance (254 nm) 0.015
Absorbance (260-400 nm) max.0.01
Water max.0.05%
Residue after evaporation max.5 ppm
Acidity (as HCOOH) max.0.001%
Peroxides (as H2O2) max.5 ppm
Fluorescence test to pass test
PFOA max.1 ng/L
PFOS max.1 ng/L
PFHxS max.1 ng/L
Assay (capillary GC) min.99.7%

We conducted a blank test using a 1000-fold concentrate of this product and confirmed that PFOA, PFHxS, and PFOS were at low levels.

Ultrapure Water

Ultrapure Water
Ultrapure Water

Methanol

Methanol
Methanol

Acetonitrile

Acetonitrile
Acetonitrile

Solid Phase Extraction Columns

Presep® PFAS

Features

  • SPE columns utilizing a filler with both reverse-phase and anion-exchange properties.
  • Two types are available. Cartridge-type and syringe-type.
  • Capable of high-efficiency recovery of 10 types of PFAS, including PFOS, PFOA, and PFHxS.

SPE Operation Examples*

Cartridge-type

Syringe-type

Column Conditioning
1) 0.1%NH3 in CH3OH 4 mL
2) CH3OH 4 mL
3) H2O 4 mL

Loading
Water + Internal standard solution and Standard solution
*Flow rate: 5 mL/min
Washing
H2O (15 mL)

Dry (N2 purge)

Extraction
0.1% NH3 in CH3OH (5 mL)
*Elution in the opposite direction to the loading direction

Extraction
0.1% NH3 in CH3OH (5 mL)

Concentration (→0.5 mL)

LC/MS/MS
Injection volume: 5 μL

*Conditions may need to be reviewed.

Additive Recovery Test for 10 PFAS*

Compound Name Abbreviation Number of
Carbon Atoms		 Recovery Rate (%)
General Reverse-
phase Column		 Presep-PFAS
Perfluorobutanoic Acid PFBA 4 0 106
Perfluorobutanesulfonic Acid PFBS 4 53 104
Perfluoropentanoic Acid PFPeA 5 8 101
Perfluorohexanoic Acid PFHxA 6 62 102
Perfluorohexanesulfonic Acid PFHxS 6 99 98
Perfluoroheptanoic Acid PFHpA 7 94 111
Perfluorooctanoic Acid PFOA 8 89 99
Perfluorooctanesulfonic Acid PFOS 8 102 99
Perfluorononanoic Acid PFNA 9 109 106
Perfluoro(2-methyl-3-oxahexanoic) Acid GenX
(HEPO-DA)		 - 63 89

*This data is an analysis example and does not guarantee the product.

Presep®-C Agri (Short)

Additive recovery test (PFOA, PFOS) using Presep®-C Agri (Short)

Sample

Ultrapure Water: for PFAS Analysis
Standard Solution: PFOS・PFOA mixture standard solution (PFOS (linear): 78 μg/L, PFOA (linear): 100 μg/L)
Internal Standard Solution: 13C-PFOS・13C-PFOA mixture standard solution (PFOS: 100 μg/L, PFOA: 100 μg/L)

  • Collection / Concentration Operation
    Water (500 mL) + Standard and Internal Standard Solution
    ▼
    Presep®-C Agri (Flow rate 5 mL/min.)
    ▼
    Washing (H2O 5 mL)
    ▼
    Dry (N2 purge)
    ▼
    Extraction (0.1%NH3 in CH3OH 5 mL)
    ▼
    Concentration (→0.5 mL)
    ▼
    LC/MS/MS
  • Column Conditioning
    1. 0.1%NH3 in CH3OH 4 mL
    2. CH3OH 4 mL
    3. H2O 4 mL
LC/MS/MS Conditions

  • Column: Wakopak® Ultra C18-3 2.0 mm×150 mm
    Eluent: A)10 mM CH3COONH4 in H2O, B)CH3CN
    LC/MS/MS: Prominence LC-20ADXR / LCMS 8030 plus

  • Gradient:

    Time (min) B conc. (%)
    0-1 25
    1-26 25-100
    26-30 100
    30-30.01 100-25
    30.01-35 25

Result

Chromatogram
Recovery Result
Monitoring Ions (m/z) Recovery Rate
Precursor Product
PFOS 498.8 80.0 100.9%
PFOA 412.9 169.1 95.0%

Product List

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Mixture Standard Solution(*A mixed standard product with a clearly defined content of linear chain.)

Internal Standards Mixture Solution(*A mixed standard product with a clearly defined content of linear chain.)

Analytical Standard(*A mixed standard product with a clearly defined content of linear chain.)

Solid-Phase Extraction Columns

HPLC Column

Delay Column

Solvents

Author: Y. Nakamura

For research use or further manufacturing use only. Not for use in diagnostic procedures.

Product content may differ from the actual image due to minor specification changes etc.

If the revision of product standards and packaging standards has been made, there is a case where the actual product specifications and images are different.

The prices are list prices in Japan.Please contact your local distributor for your retail price in your region.

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