Manual Extraction of PFAS in Drinking Water Following DIN 38407-42

Applications | 2022 | BiotageInstrumentation

Sample Preparation, Consumables, LC/MS, LC/MS/MS, LC/QQQ

Industries

Environmental

Manufacturer

Agilent Technologies, Biotage

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Summary

Significance of the Topic

Per‐ and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants widely detected in drinking water. Their strong carbon–fluorine bonds make them resistant to conventional treatment and raise human health concerns. International standards such as DIN 38407-42 require sensitive, reproducible methods for monitoring trace levels of PFAS in large water volumes.

Study Objectives and Overview

This application note describes a manual extraction workflow following DIN 38407-42 to isolate PFAS from 250–500 mL drinking water samples. Key goals are:

Validate a vacuum‐assisted SPE protocol using Biotage VacMaster and PFAS-free accessories.
Compare EVOLUTE PFAS 500 mg/6 mL and 150 mg/6 mL cartridges for recovery and reproducibility.
Demonstrate low background, minimal carryover, and compliance with a 2 ng/L Minimum Reporting Level (MRL).

Methodology and Instrumentation

Sample preparation and extraction followed these main steps:

Acidify water to pH 3 with glacial acetic acid; spike with labeled internal standards.
Condition SPE cartridges with 0.1% NH4OH in methanol, methanol, then equilibrate with reagent water.
Load samples at 5 mL/min; wash sequentially with acetate buffer and water; dry under vacuum.
Elute analytes with methanol and 0.1% NH4OH in methanol; concentrate to 1 mL via TurboVap LV.
Analyze by LC-MS/MS using Agilent 1290 Infinity II with PFC‐delay and C18 columns and an Agilent 6470 triple quadrupole in negative mode.

Main Results and Discussion

– Calibration was linear from 0.2 to 20 ppt (R² > 0.99), forced through zero.
– Target MRL of 2 ng/L achieved with recoveries of 89–106% and CVs below 10% for both cartridge sizes.
– System background tests showed all PFAS levels below one-third of the MRL after SPE and cleanup.
– Carryover after four 50 ng/L loads was negligible (<0.1 ng/L for most compounds).
– Initial demonstration of precision and accuracy at 15 ng/L confirmed recoveries within ±15% of target and CV < 10%.

Benefits and Practical Applications of the Method

– Compliant with DIN 38407-42 requirements for drinking water PFAS analysis.
– PFAS-free manifold and accessories minimize background contamination.
– Flexible cartridge formats (150 mg and 500 mg) accommodate sample volume and target range.
– High throughput: vacuum manifold supports up to 20 samples concurrently and TurboVap LV enables rapid concentration.
– Suitable for environmental monitoring labs, regulatory testing, and QA/QC in water utilities.

Future Trends and Potential Applications

Advances likely to focus on:

Automated on‐line SPE coupled directly to LC-MS/MS for higher throughput.
Miniaturized extraction devices and micro-SPE to reduce solvent use and waste.
New sorbent chemistries for broader PFAS speciation, including precursors.
High‐resolution mass spectrometry to identify unknown PFAS and transformation products.
Field‐deployable sensors and portable MS systems for on‐site screening.

Conclusion

The described manual SPE method using Biotage VacMaster, EVOLUTE PFAS cartridges, and TurboVap LV reliably quantifies trace PFAS in drinking water at sub‐ng/L levels. It meets DIN 38407-42 performance criteria, offering robust recoveries, low background, and minimal carryover for routine environmental monitoring.

Reference

Deutsche Industrie Norm DIN 38407-42: Procedures for PFAS analysis in drinking water.
ISO 21675:2019: Certified PFAS standard solutions used for spiking and calibration.

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Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 1

Manual Extraction of PFAS in Drinking Water

Following DIN 38407-42

Authors
William Jones, Biotage, Salem, NH, USA
Matthew Harden, Biotage, Salem, NH, USA

Application Note AN968

Introduction
Per- and polyfluorinated alkyl substances (PFAS) have been used abundantly since
their inception in the twentieth century and have become a closely monitored class of
compounds within environmental testing. This application note outlines a procedure for
those seeking to follow DIN 38407-42 for large volumes of water. The data presented
was generated using a Biotage® VacMaster™ vacuum manifold with a PFAS free Biotage®
VacMaster™ Large Volume Extraction (LVE) kit in conjunction with EVOLUTE® PFAS SPE
columns and a TurboVap® LV system.

Agilent

» InfinityLab PFC Delay Column, 4.6 x 30 mm, p/n 5062-8100

» ZORBAX RRHD Eclipse Plus C18, 95 Å,

2.1 x 50 mm, 1.8 µm, p/n 959757-902

Sigma-Aldrich

» Ammonium Acetate, ACS Reagent

Grade ≥ 97%, p/n 238074-25G

» Acetic Acid, Glacial, ReagentPlus®, ≥ 99% p/n A6283
Honeywell

» Water, ACS Certified, HPLC Grade, p/n AH365-4

» Methanol, Burdick & Jackson™, LC-MS Grade, p/n LC230-4
VWR

» 15 mL Polypropylene Centrifuge Tubes

with Caps, p/n 21008-670

» 250 mL Polypropylene Wide Mouth Bottles, p/n 414004-125

Equipment and Materials Used
Biotage

» Biotage® VacMaster™ 20 Sample Processing Station (with

15 mL rack), p/n 121-2015ML, fitted with polypropylene
(PFAS free) stopcocks (p/n 121-0009-PP)

» Biotage® VacMaster™ LVE Kit (PFAS)

for 1, 3, 6 mL SPE Columns (p/n 121-2190)

» EVOLUTE® PFAS 500 mg/6 mL SPE Columns, p/n 614-0050-CP

» EVOLUTE® PFAS 150 mg/6 mL SPE Columns, p/n 614-0015-CP

» TurboVap® LV Automated Solvent

Evaporation System, p/n 415000

» TurboVap® LV Multi Rack (48 Positions,

10–20 mm Tubes), p/n 414964

Wellington Laboratories

» ISO 21675:2019 Labelled Stock Solution,

1.2 mL, p/n ISO 21675-LSS

» ISO 21675:2019 Native Stock Solution,

1.2 mL, p/n ISO 21675-NSS

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 2

Analytes
Table 1. Listing of Target Analytes and Internal Standards.

Target Analyte

Acronym

CAS

Perfluorobutanoic acid

PFBA

375-22-4

Perfluoropentanoic acid

PFPeA

2706-90-3

Perfluorohexanoic acid

PFHxA

307-24-4

Perfluoroheptanoic acid

PFHpA

375-85-9

Perfluorooctanoic acid

PFOA

335-67-1

Perfluorononanoic acid

PFNA

375-95-1

Perfluorodecanoic acid

PFDA

335-76-2

Perfluorobutanesulfonic acid

PFBS

375-73-5

Perfluorohexanesulfonic acid

PFHxS

355-46-4

Perfluorooctanesulfonic acid

PFOS

1763-23-1

Perfluoroundecanoic acid1

PFUnA

2058-94-8

Perfluorododecanoic acid1

PFDoA

307-55-1

Perfluoroheptanesulfonic acid1

PFHpS

375-92-8

Perfluorodecanesulfonic acid1

PFDS

335-77-3

1H,1H,2H,2H-perfluorooctanesulfonic acid1

H4PFOS

27619-97-2

Internal Standard

Perfluoro-n-[1,2,3,4-13C4]butanoic acid

C4-PFBA

Perfluoro-n-[1,2,3,4,5-13C5]pentanoic acid

C5-PFPeA

Perfluoro-n-[1,2-13C2]hexanoic acid

C2-PFHxA

Sodium perfluoro-1-[1,2,3-13C3]hexanesulfonate

C3-PFHxS

Sodium perfluoro-1-[1,2,3-18O2]hexanesulfonate

O2-PFHxS

Perfluoro-n-[1,2,3,4-13C4]heptanoic acid

C4-PFHpA

Perfluoro-[1,2-13C4]octanoic acid

C4-PFOA

Sodium perfluoro-1-[1,2,3,4-13C4]octanesulfonate

C4-PFOS

Perfluoro-n-[13C5]nonanoic acid

C5-PFNA

Perfluoro-n-[1,2-13C2]decanoic acid

C2-PFDA

Target compounds are from the expanded list given in DIN 38407-42 Section 2.1.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 3

Solution Preparation
Ammonia/Methanol Solution
1. Add 400 μL of NH4OH for every 100 mL of methanol to

a clean beaker.

2.  Agitate to homogenize.
3.  Prepare new solution daily.
Acetate Buffer
1.  Measure out 499.5 mL of reagent water in a clean beaker.
2.  Add 0.193 g of NH4Ac.
3.  Sonicate the solution for 5 minutes until the salt is

fully dissolved.

4.  Add 570 μL of glacial acetic acid.
5.  Agitate to homogenize the solution.
Working Spiking Solution
1.  Dilute 100 μL of the native stock solution with 900 μL of

methanol to achieve a 10 ppt solution.

Summary of SPE Method
SPE Column Format
EVOLUTE® PFAS 500 mg/6 mL or EVOLUTE® PFAS 150 mg/6 mL

Sample Pre-Treatment
Adjust the pH of each sample to 3 using glacial acetic acid. Add
targets and internal standards.

Conditioning
Condition each column with 0.1 % NH4OH in methanol (10 mL)
followed by methanol (10 mL).

Equilibration
Equilibrate each column with reagent water (10 mL).

Sample Loading
Load sample at a flow rate of 5 mL/min.

Wash
Rinse the sample container with acetate buffer solution (10 mL)
and load onto the column. Repeat using reagent water (10 mL).

Dry
Dry the column for 5 minutes at a flow rate of 5 mL/min.

Elution
Rinse the sample container with methanol (5 mL) and use to
elute the analytes from the column at a flow rate of 2 mL/min.
Repeat using 0.1 % NH4OH in methanol (5 mL).

Post Extraction
Concentrate the extract to a volume of 1 mL. Add IS and mix
prior to analysis.

Note: EVOLUTE® PFAS 60 mg/3 mL columns may be used
however sample and solvent volumes should be adjusted.
Refer to DIN 38407-42 for the appropriate amounts.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 4

Sample Preparation Procedure
1. Clean all parts of the Biotage® VacMaster™ system per the

procedure given in Appendix A.

2. Set up and fill new sample containers with water;

250–500 mL are typical for this method.

3. Add glacial acetic acid to each of the sample containers to

reduce the pH to 3 (approximately 100 μL for 250 mL sample
volumes and 200 μL for 500 mL sample volumes).

4. Verify the pH of the sample is 3 using pH paper. To reduce

the possibility of contamination, a duplicate volume was
collected and adjusted to the appropriate pH and the same
volume of acid was added to the sample container.

5. Prepare for the determination of the initial sample volume by

either marking the level of the sample on the container or by
weighing the sample container.

6. Add 20 μL of the undiluted Labeled Stock Solution to each

of the sample containers. If desired, fortify a sample using
target analytes: the addition of 125 μL or 37.5 μL of the native
stock solution will yield either 50 ppt or 15 ppt concentra-
tions respectively, while the addition of 50 μL of the working
spiking solution will yield a 2 ppt concentration. If the mixes
used were different than the ones outlined in this note,
adjust the concentration or spiking amounts as needed.

7. Load the desired EVOLUTE® PFAS columns onto the Biotage®

VacMaster™. Seal any unused positions using VacMaster Port
Sealing Plugs (p/n 121-0005)

8. Rinse each column with 10 mL of 0.1 % NH4OH in methanol

and apply vacuum at 10 mL/min to pull it to waste. Do not
allow the sorbent to go dry.

9. Rinse each column with 10 mL of methanol and apply

vacuum at 10 mL/min to pull it to waste. Do not allow the
sorbent to go dry.

10. Rinse each column with 10 mL of reagent water and apply

vacuum at 10 mL/min to send it to waste. Do not allow the
water level to drop below the top of the packing.

11. Using the Biotage® VacMaster™ LVE Kit, place one end of

the cleaned tubing into the bottom of each of the sample
containers, and secure in position using the clips provided.

12. Load the samples onto the columns using a flow rate of

5 mL/min.

13. Once the sample has been fully loaded, rinse the sample

containers using 10 mL of acetate buffer solution, swirl to
ensure the full rinsing of the container, and load the aliquot
onto the column at a rate of 5 mL/min.

14. Rinse the sample containers using 10 mL of reagent water,

swirl to ensure the full rinsing of the container, and load the
aliquot onto the column at a rate of 5 mL/min.

15. Dry the column for 5 minutes at a rate of 5 mL/min.
16. Load 15 mL centrifuge tubes into the rack corresponding to

each of the column positions and load into the VacMaster.

17. Rinse each sample container using 5 mL of methanol and

swirl to ensure the full rinsing of the container. Load the
aliquot through the appropriate column and collect at a
dropwise rate.

18. Rinse each sample container using 5 mL of 0.1% NH4OH

in methanol and swirl to ensure the full rinsing of the
container. Load the aliquot through the appropriate column
and collect at a dropwise rate.

19. Determine the initial sample volume by either using a gradu-

ated cylinder and filling the sample container to the original
mark or by taking an additional weight of the container.

20. Transfer the centrifuge tubes to the TurboVap® LV system and

concentrate the samples to just under 1 mL using nitrogen
according to the parameters in Table 2.

21. Bring the final extract to 1 mL and transfer to an

autosampler vial.

22. Load the extract onto a calibrated LC-MS/MS system and

process using the conditions given in the below sections.

Table 2. TurboVap® LV Concentration Protocol.

Bath Temp:

60 ˚C

Evaporation Mode

Method (Ramp Gradient)

Manifold Setup

48 positions

Rack Row Height

120 mm*

Step 1:

1.5 L/min for 20 min

Step 2:

3.0 L/min for 15 min

Step 3:

3.5 L/min for 45 min

*The nozzle position was adjusted such that it was as far to the right as

possible to give the user a clear view of the vortex within the tube.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 5

LC-MS/MS Conditions
Agilent 1290 Infinity II LC System

» 1290 Infinity II Multicolumn Thermostat, G7116B

» 1290 Infinity II Multisampler, G7167B

» 1290 Infinity II High Speed Pump, G7120A

» InfinityLab PFC-free HPLC Conversion Kit, 5004-0006

Columns

» InfinityLab PFC Delay Column, 4.6 x 30 mm, p/n 5062-8100

» ZORBAX RRHD Eclipse Plus C18, 95 Å,

2.1 x 50 mm, 1.8 µm, p/n 959757-902

Mobile Phases

» A: 20 mM Ammonium Acetate in Water

» B: Methanol

Table 3. LC Gradient.

Time (min)

0.50

95.00

5.00

3.00

60.00

40.00

16.00

20.00

80.00

18.00

20.00

80.00

20.00

5.00

95.00

20.50

0.00

100.00

25.00

0.00

100.00

26.00

5.00

95.00

» Flow Rate: 0.2 mL/min

» Injection Volume: 5 μL

» Column Temperature: 50 ˚C

Agilent 6470 MS/MS, G6470B

» Gas Temperature: 230 ˚C

» Gas Flow: 4 L/min

» Nebulizer: 20 psi

» Sheath Gas Temperature: 375 ˚C

» Sheath Gas Flow: 12 L/min

» Capillary Voltage (Positive): 3500 V

» Capillary Voltage (Negative): 3500 V

» Nozzle Voltage (Positive): 500 V

» Nozzle Voltage (Negative): 0 V

For a complete listing of MRM Transitions, see Appendix B

Results
System Calibration
For the work being done here, a total of six points were used
in the calibration covering a range of 0.2-20 ppt. The lowest
three points were below the calculated MRL. The curve was
forced through zero and achieved excellent linearity across the
calibration range.

PFBS

PFHxS

Figure 1. Calibration curves for PFBS and PFHxS. Calibration curves for

the remaining target analytes in Table 1 are shown in Appendix C.

Determination of the Minimum Reporting

Level (MRL) and Detection Limits (DL)
A target MRL of 2 ng/L was selected and at least seven replicate
laboratory fortified blanks (LFBs) were created and run at that
concentration. Figure 2 below illustrates the results of this test
for both the 150 mg and 500 mg columns using 250 mL sample
volumes; all compounds were recovered within 15% of the
spiked amount and had less than 10% CV.

Figure 2. MRL and DL Recoveries. Those compounds with an asterisk were

used in salt form.

The data for individual compounds is shown in Appendix D.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 6

Demonstration of Low System Background
An investigation into the background of the complete process
was done in three steps. The first step was to run blank
injections of methanol on the analytical system (system blank).
The second step was to load centrifuge tubes containing a
similar volume of methanol as would result from the extraction
process onto the evaporation system, allowing them to
concentrate and then run on the analytical system (evaporation
blank). The third and final step was to create a full Laboratory
Reagent Blank (LRB), extract and concentrate it, and run it on
the analytical system. By separating the process into three
steps it becomes easier to determine what, if any, contribution
to the overall background each of the steps has. The result of
these tests are given in Appendix E and selected data are shown
below in Figures 3–5.

Figure 3. Contribution of the TurboVap® LV to the PFAS Background.

Those compounds with an asterisk were used in salt form.

Figure 4. PFAS Background for full LRB using EVOLUTE® PFAS 500 mg/6 mL

columns. Those compounds with an asterisk were used in salt form.

Figure 6. Initial Demonstration of Accuracy (15 ng/L, n=4).

Those compounds with an asterisk were used in salt form.

Figure 7. Initial Demonstration of Precision (15 ng/L, n=4). Those

compounds with an asterisk were used in salt form.

Figure 5. PFAS Background for full LRB using EVOLUTE® PFAS 150 mg/6 mL

columns. Those compounds with an asterisk were used in salt form.

For those results which were generated using only the analytical
system, all target analytes were N.D. (unable to be separated
from the noise in the baseline) and so were not listed out in the
previous tables.

When examining the data resulting for both the TurboVap® LV
and the full LRB tests (which includes the Biotage® VacMaster™
manifold, PFAS Free Large Volume Loading Kit, and the
EVOLUTE® cartridges as well as the TurboVap® LV) there are clear
indications of the presence of a PFAS background. However,
even at the highest concentrations detected, all levels are much
lower than the 1/3 MRL limit indicating that the background is
acceptable and will not interfere with future sample runs.

Initial Demonstration of Precision

and Accuracy (IDP, IDA)
To determine the precision and accuracy of the sample prepara-
tion process, four LFB samples were prepared at concentrations
of 15 ppt. The data is given in Appendix F and illustrated in
Figures 6 and 7.

The results show that the average recovery for each target
analyte was within 15% of the nominal value and that the
coefficient of variation (CV) for each analyte fell under 10%
on average.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 7

Examination of System Carryover
To simulate an influent sample, four LFB samples were
created with concentrations which were above the range of
the calibration curve. These samples were extracted, and
the cleanup procedure given in Appendix A was run three
times. To ensure that the system background was adequately
reduced, a set of four LRB samples were extracted immediately
afterwards and analyzed. The LRB data is presented in
Appendix G and illustrated in Figure 8.

Figure 8. Results of carryover study following four, 50 ng/L LFB samples

using EVOLUTE® PFAS 500 mg/6 mL columns. Those compounds with an

asterisk were used in salt form.

Conclusion
With the scrutiny being given to the presence of PFAS
compounds in the environment, it is essential to find reliable
products which can meet the requirements of DIN 38407-42.
This application note has shown that the VacMaster™ vacuum
manifold with PFAS free accessories, EVOLUTE® PFAS SPE
columns and the TurboVap® LV can be used to easily meet and
exceed the demands of the method.

Ordering Information

Part Number

Description

Qty

121-2015ML

Biotage® VacMaster™ 20 Sample Processing

Station With 15 mm Rack

121-2190

Biotage® VacMaster™ LVE Kit (PFAS) for 1, 3,

6 mL SPE Columns

121-0009-PP

Polypropylene (PFAS) Stopcocks

614-0050-CP EVOLUTE® PFAS 500 mg/6 mL columns

614-0015-CP

EVOLUTE® PFAS 150 mg/6 mL columns

614-0006-BP EVOLUTE® PFAS 60 mg/3 mL columns

415000

TurboVap® LV Automated Solvent

Evaporation System

414964

TurboVap® LV Multi Rack (48 Positions,

10–20 mm Tubes)

The graph shown in Figure 8 shows a clear indication that the
cleaning procedure in Appendix A was successful in reducing
the background of PFAS compounds to below the 1/3 MRL limit.
For further reductions in the background, additional cleaning
steps could be employed.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 8

Appendix A

Biotage® VacMaster™ Cleaning Procedure

For the best results, it is recommended that this procedure be
completed before the use of the VacMaster™ each day and at the
end of each extraction prior to proceeding with the next set of
samples.

1. Ensure that a column and column adapter is installed onto

each VacMaster™ position slated to be cleaned.

2. Fill a clean beaker with 50 mL of methanol and place no more

than four of the LVE Kit lines into the beaker.

3. Apply vacuum to the manifold and pull the methanol through

the positions into the waste container.

4. Remove the column and discard.
5. Using methanol in a squeeze bottle, clean the exterior of the

LVE Kit’s lines, the column adapters, the stopcock, and the
metal cannula. Discard all rinsate.

6. Repeat this up to three times for all positions which

require cleaning.

Note: In situations where the previous sample was highly
concentrated, the above cleaning procedure may need to be
repeated multiple times. If there is concern regarding potential
carryover contamination regardless of the cleaning procedure,
a laboratory reagent blank should be run in that position to
ensure its cleanliness.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 9

Appendix B

MRM Transitions

Table 4. MRM Transitions for Agilent 6470 MS/MS.

Cpd Name

ISTD?

Prec

Ion

MS1 Res

Prod

Ion

MS2 Res

Frag

(V)

Cell Acc

(V)

Ret Time

(min)

Ret

Window

Polarity

H4PFOS

427

Unit/Enh (6490)

406.8

Unit/Enh (6490)

125

13.3

1.37

Negative

H4PFOS

427

Unit/Enh (6490)

80.9

Unit/Enh (6490)

125

13.3

1.37

Negative

C3-PFHxS

402

Unit/Enh (6490)

100

11.7

1.5

Negative

C4-PFBA

217

Unit/Enh (6490)

172

Unit/Enh (6490)

5.1

1.45

Negative

C4-PFHpA

367

Unit/Enh (6490)

322

Unit/Enh (6490)

11.6

1.2

Negative

C5-PFHxA

318

Unit/Enh (6490)

273

Unit/Enh (6490)

9.7

1.14

Negative

C5-PFPeA

268

Unit/Enh (6490)

223

Unit/Enh (6490)

7.4

1.55

Negative

C6-PFDA

519

Unit/Enh (6490)

474

Unit/Enh (6490)

16.2

1.65

Negative

C8-PFOA

421

Unit/Enh (6490)

376

Unit/Enh (6490)

13.4

1.38

Negative

C8-PFOS

507

Unit/Enh (6490)

100

1.53

Negative

C9-PFNA

472

Unit/Enh (6490)

427

Unit/Enh (6490)

14.9

1.52

Negative

PFBA

213

Unit/Enh (6490)

168.9

Unit/Enh (6490)

5.1

1.48

Negative

PFBS

298.9

Unit/Enh (6490)

98.9

Unit/Enh (6490)

100

7.9

1.41

Negative

PFBS

298.9

Unit/Enh (6490)

100

7.9

1.41

Negative

PFDA

513

Unit/Enh (6490)

469

Unit/Enh (6490)

16.2

1.65

Negative

PFDA

513

Unit/Enh (6490)

218.7

Unit/Enh (6490)

100

16.2

1.65

Negative

PFDoA

613

Unit/Enh (6490)

569

Unit/Enh (6490)

18.2

1.84

Negative

PFDoA

613

Unit/Enh (6490)

268.7

Unit/Enh (6490)

100

18.2

1.84

Negative

PFDS

599

Unit/Enh (6490)

100

17.15

1.75

Negative

PFDS

599

Unit/Enh (6490)

100

17.15

1.75

Negative

PFHpA

362.9

Unit/Enh (6490)

319

Unit/Enh (6490)

11.6

1.2

Negative

PFHpA

362.9

Unit/Enh (6490)

169

Unit/Enh (6490)

11.6

1.2

Negative

PFHpS

448.9

Unit/Enh (6490)

98.7

Unit/Enh (6490)

100

13.5

1.39

Negative

PFHpS

448.9

Unit/Enh (6490)

79.7

Unit/Enh (6490)

100

13.5

1.39

Negative

PFHxA

313

Unit/Enh (6490)

268.9

Unit/Enh (6490)

9.7

1.12

Negative

PFHxA

313

Unit/Enh (6490)

119

Unit/Enh (6490)

9.7

1.12

Negative

PFHxS

398.9

Unit/Enh (6490)

100

11.7

1.5

Negative

PFHxS

398.9

Unit/Enh (6490)

100

11.7

1.5

Negative

PFNA

463

Unit/Enh (6490)

419

Unit/Enh (6490)

14.9

1.52

Negative

PFNA

463

Unit/Enh (6490)

219

Unit/Enh (6490)

14.9

1.52

Negative

PFOA

413

Unit/Enh (6490)

369

Unit/Enh (6490)

13.4

1.38

Negative

PFOA

413

Unit/Enh (6490)

169

Unit/Enh (6490)

13.4

1.38

Negative

PFOS

498.9

Unit/Enh (6490)

100

1.53

Negative

PFOS

498.9

Unit/Enh (6490)

100

1.53

Negative

PFPeA

263

Unit/Enh (6490)

218.9

Unit/Enh (6490)

7.4

1.77

Negative

PFUnA

563

Unit/Enh (6490)

519

Unit/Enh (6490)

17.2

1.75

Negative

PFUnA

563

Unit/Enh (6490)

269

Unit/Enh (6490)

100

17.2

1.75

Negative

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 10

Appendix C

Calibration Curves

Figure 9. Calibration curves for the target analytes in Table 1, covering a

concentration range of 0.2-20 ppt.

PFBA

PFHpS

H4PFOS

PFOA

PFOS

PFPeA

PFHxA

PFHpA

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 11

PFNA

PFDA

PFDS

PFUnA

PFDoA

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 12

Appendix D

MRL and DL Data

Table 6. MRL and DL Recoveries for EVOLUTE® PFAS 150 mg/6 mL columns.

Conc.

(ng/L)

x̅

(ng/L)

x̅

(%)

(ng/L)

(%)

(ng/L)

PFBA*

1.77

1.88

1.83

1.87

1.94

1.83

1.86

1.79

1.83

1.85

104

0.05

2.56

0.14

PFPeA

2.00

1.96

1.92

1.96

2.05

1.97

1.93

1.86

1.96

1.95

0.05

2.79

0.16

PFBS

2.00

1.87

1.76

1.84

1.73

1.77

1.81

1.73

1.75

1.78

0.05

2.83

0.15

PFHxA

2.00

2.09

2.00

2.04

2.10

2.03

2.09

1.98

2.08

2.05

103

0.05

2.20

0.14

PFHpA

2.00

2.08

1.96

1.98

1.91

2.04

1.95

2.01

1.99

100

0.06

2.76

0.17

PFHxS*

1.90

1.75

1.83

1.80

1.85

1.66

1.74

1.77

1.74

1.77

0.06

3.34

0.18

PFHpS*

1.91

1.77

1.78

1.85

1.79

1.64

1.66

1.69

1.64

1.73

0.08

4.69

0.24

H4PFOS*

1.90

1.91

1.84

1.97

1.92

2.05

2.06

2.01

2.11

1.98

104

0.09

4.58

0.27

PFOA

2.00

1.96

1.99

2.01

2.08

1.97

2.05

1.91

1.97

1.99

100

0.05

2.59

0.15

PFOS*

1.92

2.00

1.89

1.93

2.01

1.95

1.98

1.96

102

0.04

1.99

0.12

PFNA

2.00

2.08

1.94

2.02

2.01

2.04

2.08

2.11

2.02

2.03

102

0.05

2.59

0.16

PFDA

2.00

1.99

1.89

1.96

1.99

1.91

2.03

2.07

2.04

1.98

0.06

3.12

0.19

PFDS

2.00

1.92

2.08

1.81

2.04

2.01

1.93

2.04

1.90

1.97

0.09

4.61

0.27

PFUnA

2.00

2.09

1.97

1.93

1.95

1.89

1.97

1.95

1.98

1.97

0.06

2.94

0.17

PFDoA

2.00

2.08

1.91

2.02

2.05

2.02

2.03

2.04

2.02

101

0.05

2.52

0.15

*Analytes were used in salt form and calculated concentrations were corrected to compensate where needed.

Table 5. MRL and DL Recoveries for EVOLUTE® PFAS 500 mg/6 mL columns.

Conc.

(ng/L)

x̅

(ng/L)

x̅

(%)

(ng/L)

(%)

(ng/L)

PFBA*

1.77

1.67

1.71

1.67

1.68

1.81

1.60

1.80

1.71

0.08

4.43

0.24

PFPeA

2.00

1.85

1.83

1.92

1.97

1.88

1.75

1.91

1.87

0.07

3.81

0.22

PFBS

2.00

1.73

1.90

1.82

1.70

1.73

1.65

1.95

1.78

0.11

6.12

0.34

PFHxA

2.00

1.80

1.92

1.89

1.80

1.98

1.75

1.92

1.87

0.08

4.50

0.26

PFHpA

2.00

1.96

2.06

2.04

1.94

2.01

1.80

2.08

1.99

0.09

4.75

0.30

PFHxS*

1.90

1.85

1.78

1.77

1.70

1.82

1.73

1.77

0.05

2.84

0.16

PFHpS*

1.91

1.90

1.86

1.65

1.92

1.51

1.73

1.78

0.16

8.79

0.49

H4PFOS*

1.90

1.80

1.87

1.88

1.86

1.87

1.68

1.86

1.83

0.07

4.02

0.23

PFOA

2.00

1.80

1.86

1.93

1.91

1.94

1.67

1.94

1.86

0.10

5.34

0.31

PFOS*

1.92

1.96

1.89

1.79

1.89

1.92

1.69

1.89

1.86

0.09

4.98

0.29

PFNA

2.00

1.88

1.92

1.95

1.90

1.94

1.79

2.07

1.92

0.08

4.30

0.26

PFDA

2.00

1.87

1.89

1.87

1.83

2.01

1.79

2.01

1.89

0.09

4.55

0.27

PFDS

2.00

2.10

2.06

1.95

2.14

1.70

1.64

1.93

0.19

9.98

0.61

PFUnA

2.00

1.89

1.91

1.90

1.81

1.88

1.75

1.94

1.87

0.07

3.51

0.21

PFDoA

2.00

1.85

1.96

1.81

2.00

1.75

1.96

1.90

0.10

5.04

0.30

*Analytes were used in salt form and calculated concentrations were corrected to compensate where needed.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 13

Appendix E

PFAS Background Study

Table 7. Results of PFAS Background Study for EVOLUTE® PFAS 500 mg/6 mL columns (recoveries in ng/L).

TurboVap® LV

Laboratory Reagent Blanks

Replicate

PFBA*

0.00

0.10

0.05

0.04

0.09

0.06

PFPeA

0.02

0.03

0.06

0.02

0.03

0.04

0.02

0.04

PFBS

0.01

0.00

0.01

0.00

0.01

0.00

0.06

PFHxA

0.01

0.02

0.00

0.01

0.00

0.02

0.01

0.02

PFHpA

0.00

PFHxS*

0.00

0.01

0.00

0.01

PFHpS*

0.00

0.02

0.00

H4PFOS*

0.02

0.00

0.01

0.05

0.06

0.07

PFOA

0.02

0.00

0.03

0.00

0.01

0.00

PFOS*

0.00

0.03

0.00

0.02

0.01

0.02

0.01

PFNA

0.00

0.01

0.00

0.02

0.00

0.01

0.00

PFDA

0.00

0.02

0.00

PFDS

0.00

PFUnA

0.00

PFDoA

0.00

*Analytes were used in salt form and calculated concentrations were corrected to compensate where needed.

Table 8. Results of PFAS Background Study for EVOLUTE® PFAS 150 mg/6 mL columns (recoveries in ng/L).

TurboVap® LV

Laboratory Reagent Blanks

Replicate

PFBA*

0.06

0.02

0.01

0.00

0.11

0.09

0.10

PFPeA

0.03

0.02

0.05

0.06

0.04

PFBS

0.01

0.00

0.01

PFHxA

0.02

0.01

0.00

0.03

0.02

PFHpA

0.00

PFHxS*

0.01

0.00

0.01

PFHpS*

0.00

H4PFOS*

0.01

0.00

0.03

0.04

0.02

PFOA

0.00

0.02

0.03

0.00

0.05

0.00

PFOS*

0.00

0.01

0.00

PFNA

0.00

0.01

0.00

0.01

0.00

PFDA

0.00

0.02

0.00

0.02

PFDS

0.00

0.01

0.00

PFUnA

0.00

0.02

0.00

PFDoA

0.00

0.06

0.00

*Analytes were used in salt form and calculated concentrations were corrected to compensate where needed.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 14

Appendix F

IDP and IDA Data

Table 9. Results of IDP and IDA for EVOLUTE® PFAS 500 mg/6 mL columns (15 ng/L, n=4).

Replicate

1 (%)

2 (%)

3 (%)

4 (%)

x̅ (%)

s (%)

CV (%)

PFBA*

93.97

93.52

97.66

94.56

94.93

1.87

1.97

PFPeA

91.10

99.84

99.34

92.16

95.61

4.62

4.83

PFBS

88.73

88.20

91.76

86.48

88.79

2.20

2.47

PFHxA

94.83

95.12

99.13

95.85

96.23

1.98

2.06

PFHpA

104.38

106.43

104.54

106.18

105.38

1.07

1.02

PFHxS*

95.20

99.75

101.57

95.96

98.12

3.04

3.10

PFHpS*

89.31

87.18

98.22

79.57

88.57

7.67

8.66

H4PFOS*

96.43

102.56

100.83

101.53

100.34

2.70

2.69

PFOA

94.28

94.77

96.59

92.79

94.61

1.56

1.65

PFOS*

91.58

93.17

98.48

89.66

93.22

3.79

4.06

PFNA

93.76

98.27

100.96

96.89

97.47

2.99

3.07

PFDA

96.19

91.59

101.20

100.51

97.38

4.45

4.57

PFDS

96.50

102.88

108.47

98.56

101.60

5.29

5.21

PFUnA

88.89

85.05

87.96

90.74

88.16

2.37

2.69

PFDoA

96.65

99.00

102.74

98.79

99.30

2.53

2.55

*Analytes were used in salt form and calculated concentrations were corrected to compensate where needed.

Table 10. Results of IDP and IDA for EVOLUTE® PFAS 150 mg/6 mL columns (15 ng/L, n=4).

Replicate

1 (%)

2 (%)

3 (%)

4 (%)

x̅ (%)

s (%)

CV (%)

PFBA*

102.37

101.69

101.80

103.26

102.28

0.72

0.70

PFPeA

101.89

102.16

101.32

100.30

101.42

0.82

0.81

PFBS

99.30

102.15

99.56

102.63

100.91

1.72

1.71

PFHxA

100.58

103.25

99.56

100.27

100.92

1.61

1.60

PFHpA

102.78

102.88

102.64

102.10

102.60

0.35

0.34

PFHxS*

97.07

98.52

98.87

97.40

97.96

0.86

0.88

PFHpS*

91.57

92.08

90.92

93.18

91.94

0.95

1.04

H4PFOS*

99.40

99.12

104.89

102.46

101.47

2.74

2.70

PFOA

104.83

105.70

104.59

106.65

105.44

0.94

0.89

PFOS*

101.18

103.31

101.24

102.55

102.07

1.04

1.02

PFNA

102.52

103.28

101.34

101.57

102.18

0.90

0.88

PFDA

102.85

104.63

101.29

103.65

103.10

1.41

1.37

PFDS

105.46

102.18

103.54

106.38

104.39

1.89

1.81

PFUnA

98.55

97.67

97.27

98.90

98.10

0.76

0.77

PFDoA

105.74

103.29

103.54

105.36

104.48

1.25

1.19

*Analytes were used in salt form and calculated concentrations were corrected to compensate where needed.

Manual Extraction of PFAS in Drinking Water Following DIN 38407-42 | Page 15

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Appendix G

Carryover Data

Table 11. Results of carryover study following four, 50 ng/L LFB samples using EVOLUTE® PFAS 500 mg/6 mL columns.

Replicate

(ng/L)

x̅

(ng/L)

PFBA*

0.11

0.09

PFPeA

0.04

PFBS

0.02

0.01

0.02

0.01

0.02

PFHxA

0.02

0.03

PFHpA

0.00

PFHxS*

0.02

0.00

0.02

0.01

PFHpS*

0.00

H4PFOS*

0.04

PFOA

0.09

0.04

0.07

0.00

0.05

PFOS*

0.04

0.03

0.04

PFNA

0.00

PFDA

0.02

PFDS

0.03

0.00

0.01

PFUnA

0.00

0.03

0.01

PFDoA

0.00

*Analytes were used in salt form and calculated concentrations were corrected to compensate where needed.

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