EPA Method 1633 Instrumentation Guide

LC-MS/MS for PFAS Analysis

EPA Method 1633A is the U.S. EPA’s multi-laboratory validated method for measuring 40 per- and polyfluoroalkyl substances (PFAS) in wastewater, surface water, groundwater, landfill leachate, soil, sediment, biosolids and fish tissue. The EPA Office of Water developed it with the U.S. Department of Defense, and the December 2024 revision supersedes all earlier versions of Method 1633. EPA recommends it for PFAS monitoring under NPDES permits.

A photo of a refurbished Waters LC-MS system for EPA METHOD 1633 that links to a catalog of Liquid Chromatography-Mass Spectrometry equipment.

Aqueous samples are extracted by solid-phase extraction (SPE) and cleaned up with carbon. Solids are extracted into basic methanol, and tissue into potassium hydroxide and acetonitrile followed by basic methanol, before the same SPE and carbon cleanup. Extracts are analyzed on a triple quadrupole LC-MS/MS in negative electrospray, multiple reaction monitoring (MRM) mode, and isotopically labeled standards added before extraction correct each result for losses during preparation.

Read EPA Method 1633A.

Looking for an LC-MS/MS system for EPA Method 1633A? Browse refurbished LC-MS systems or request a configuration quote.

EPA Method 1633A Summary

Item

Detail

Method

EPA Method 1633, Revision A, December 2024 (EPA 820-R-24-007)

Analytes

40 PFAS across nine classes, including PFCAs, PFSAs, fluorotelomer sulfonates, sulfonamides and ether acids such as HFPO-DA (GenX)

Matrices

Wastewater, surface water, groundwater, landfill leachate, soil, sediment, biosolids, fish and shellfish tissue

Technique

WAX solid-phase extraction with carbon cleanup, then isotope dilution LC-MS/MS on a triple quadrupole (negative ESI, MRM)

Sample and solvent

500 mL aqueous (100 mL leachate), 5 g soil or sediment, 0.5 g biosolids, 2 g tissue; solids extracted into basic methanol

Injection

2.0 µL default, identical for all standards, samples and QC

Working range

At least six calibration standards (linear) or seven (second-order), with the lowest at or below the lab’s LOQ

MDL

Example pooled MDLs for PFOS: 0.63 ng/L (aqueous), 0.07 ng/g (solids); each lab sets its own

Extraction and analysis time

12.0-minute LC gradient program per injection; the method does not state an extraction time

Labs may add PFAS beyond the 40 listed when authentic standards are available (Section 1.6). EPA recommends Method 1633A for NPDES monitoring; it was proposed for 40 CFR Part 136 in December 2024.

Instrument requirements

Method 1633A specifies a UHPLC or HPLC system coupled to a triple quadrupole mass spectrometer. The settings below are the method’s example conditions; equivalent columns and instruments are allowed if they meet the method’s performance criteria.

Setting

Method 1633A requirement

Mass spectrometer

Triple quadrupole, at least 10 scans across each peak

Ionization

Negative electrospray (ESI−)

Acquisition

Multiple reaction monitoring (MRM), unit mass resolution

LC system

UPLC or HPLC

Analytical column

C18, 1.7 µm, 50 × 2.1 mm (Waters ACQUITY UPLC BEH or equivalent)

Guard column

Phenomenex Kinetex EVO C18 or equivalent

Delay column

Purospher STAR RP-18 endcapped, 3 µm, Hibar RT 50-4 or equivalent

Column temperature

40 °C

Mobile phase A

Acetonitrile

Mobile phase B

2 mM ammonium acetate in 95:5 water/acetonitrile

Gradient

About 12 minutes at 0.35–0.40 mL/min; up to 1,100 bar

Mass calibration

At least annually, or as the manufacturer recommends

The method lists a trap/delay column with the LC equipment and notes that LC system components, as well as the mobile phase, may contain many of the analytes in this method.

Know the configuration you need? Request an EPA 1633A LC-MS/MS quote.

What to look for in a refurbished LC-MS/MS system

The right refurbished system combines the required hardware with evidence that it performs reliably. Use these checks when comparing systems.

System area

Method 1633A need

What to check

Mass spectrometer

Triple quadrupole, MRM, unit mass resolution, at least 10 scans per peak

Mass calibration within the past year and a passing instrument sensitivity check at the lab’s LOQ

Ion source

Negative electrospray

Operation in negative ESI mode

LC pump

12.0-minute gradient at 0.35–0.40 mL/min, column at 40 °C

Pressure rating compared with the method’s 1,100 bar maximum

Autosampler

Same injection volume for every standard, sample and QC

Consistent injection volume across the analytical sequence

Columns

C18 analytical, guard and trap/delay columns

Trap/delay column included in the LC configuration

PFAS background

Instrument blanks below each analyte’s MDL equivalent

Instrument blank results, run at the start of each sequence and after high-concentration samples

Documentation

Mass calibration at least annually

Mass calibration records

Need help comparing systems? Tell our team about your sample matrices, reporting limits and preferred platform. Talk to an instrument specialist or call (844) AMP-TECH.

Example LC-MS/MS configurations

The platforms below are examples that may be configured for EPA Method 1633A. The method names the Waters Xevo TQ-S micro “or equivalent” as its example but doesn’t require a specific brand or model, so the choice can reflect your budget, platform preference and service needs.

Platform

Configuration for Method 1633A

Key Benefits for EPA 1633A

Waters Xevo TQ-S micro

ACQUITY I-Class UPLC

The example instrument named in Method 1633A

Thermo Scientific TSQ Quantis

Vanquish UHPLC

Triple quadrupole designed for targeted quantitation

Agilent 6490

1200/1260 Infinity or 1260 Infinity II

iFunnel technology, including Agilent Jet Stream, for more efficient ion sampling

Agilent 6460

1260 HPLC

Agilent Jet Stream technology at a lower purchase price

Agilent Ultivo

1260 Infinity II

Compact, stackable triple quadrupole design

Some listed systems ship with LC front ends or detectors Method 1633A doesn’t use, but our team can help you plan an EPA Method 1633A configuration. We’ll review the LC front end, columns and trap/delay column with you before you buy.

Don’t see the right configuration in the store? Tell us what you need, and we’ll check the available options.

Choosing a configuration

Start with your sample types and reporting limits.

  • Sample types: aqueous, solid and tissue samples all need SPE and carbon cleanup; solids and tissue are extracted first, then go through the same cleanup.
  • Example configuration: the method names the Waters Xevo TQ-S micro and an Acquity UPLC BEH C18 column, each “or equivalent.”
  • Delay column: plan for a trap/delay column in the LC system, as the method lists.
  • Reporting limits: each lab sets its own MDLs and LOQs and must pass the instrument sensitivity check at its LOQ before each sequence. Browse refurbished LC-MS systems.

Amptius Certified Refurbished Instruments

AMP Tech offers refurbished analytical instruments and can help you configure a refurbished LC-MS/MS system for EPA Method 1633A. Amptius Certified refurbished instruments go through a six-stage certification process, including repair, analytical testing, and documentation before shipment, giving your lab a lower-cost alternative to buying new.

Certified instruments include a 6-month limited warranty covering parts and labor for covered defects in materials or workmanship.

AMP Guard Service Plans

For support beyond the warranty, AMP Guard offers optional service plans with remote support, service facility repair, and on-site options. Coverage depends on the plan and instrument.

Request a quote with your sample volume, confirmation approach, and preferred platform. Our documentation and technical support can help your team prepare for method validation and ongoing QC.

Sell or Trade in your lab equipment

Upgrading your lab or clearing surplus equipment? AMP Tech buys GC/MS, LC/MS and triple quad, HPLC, ICP-OES and ICP-MS, and FTIR and spectroscopy systems, along with supporting lab equipment. We buy everything from a single instrument to an entire lab, anywhere in the country.

You get a firm, no-obligation offer within 48 hours with no fees or commission. Our team handles decommissioning, packing, and removal, and you can apply your equipment’s value toward an Amptius Certified instrument.

Sell your equipment or check your trade-in value.

Sources

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