T-4-132 – Per- and polyfluoroalkyl substances (PFAS) standard for commercial biosolids imported or sold in Canada as fertilizers

1. Purpose

The purpose of this document is to provide guidance to importers and domestic producers of commercial biosolids on the interim standard for per- and polyfluoroalkyl substances in biosolids imported or sold in Canada as fertilizers or supplements. The CFIA's standard is part of a broader Government of Canada response intended to reduce human and environmental exposure to PFAS and PFAS-containing products from the point of manufacture to their disposal (product life cycle approach).

Per- and polyfluoroalkyl substances (PFAS) are a group of over 4,700 human-made substances that are used in firefighting foams, textiles (including carpets, furniture, and clothing), cosmetics, and food packaging. Due to their widespread use in households and industrial applications they can be found in our soil, air, water and in the waste stream, including municipal biosolids. PFAS are contaminants of concern due to their inherent persistence, mobility in the soil and potential for negative effects on human health and the environment.

2. Product coverage

The interim PFAS standard applies to commercial biosolids, including both those that meet the definition of municipal biosolids on the List of primary fertilizer and supplement materials and are exempt from registration under the Fertilizers Act as well as biosolids that do not meet the definition and therefore require registration.

Municipal biosolids (specify grade) are defined on the list of primary fertilizer and supplement materials as:

Solid, semi-solid or liquid material comprised of septage or municipal sewage sludge, or both, freed from grit and coarse solids, which have been subjected to physical, chemical or biological treatment, or a combination of these treatments, sufficient to mitigate against the presence and effect of generally detrimental or serious injurious substances that may be associated with untreated forms of this material.

Final products that are mixtures of commercial biosolids and other fertilizer or supplement materials are currently not covered by the standard. Similarly, other waste materials such as composts, anaerobic digestates, ash, pulp and paper sludges, source separated organics, etc., are not currently covered by the interim PFAS standard.

3. Standard

To be imported into or sold in Canada, biosolids represented as commercial fertilizers must contain less than 50 parts per billion (ppb) of perfluorooctane sulfonate (PFOS) on a dry weight basis. PFOS is used as an indicator of PFAS contamination.

4. Demonstrating compliance

To demonstrate compliance with the standard, a laboratory report (also known as a certificate of analysis) showing PFOS testing results and an accompanying attestation form are required. Documentation requirements (certificate of analysis and attestation) are described below.

When documentation will be verified

At import:

Requirements are written in the CFIA's Automated Import Reference System (AIRS) under HS Codes: 38.25.20.61 (Sewage sludge for fertilizer or supplement use), 38.25.10.61 (Municipal Waste for fertilizer or supplement use) and 31.05.90.61.985 (Fertilizer or supplement comprised of septage and/or sewage sludge that has been treated to reduce pathogens)
Documentation is verified before the shipment is cleared for entry

In the Canadian marketplace (through CFIA inspection):

Imported and domestically generated biosolids sold in Canada may be inspected by the CFIA at any time
To verify compliance with the interim standard for PFAS, CFIA inspectors will review the required certificate of analysis and attestation form

Documentation requirements

The responsible party is required to maintain valid documentation that demonstrates compliance with the interim PFAS standard at all times. Shipments that fail to meet the requirements will not be cleared for import and products inspected in Canada may be subject to compliance and enforcement activities: detention, order to remove/re-export, safe disposal.

Certificate of analysis

The laboratory must be accredited by a body that is a signatory of the International Laboratory Accreditation Cooperation Mutual Recognition Arrangement (ILAC MRA) and have draft US EPA method 1633 (PDF) listed on their scope of accreditation for biosolids.
- A list of laboratories accredited for draft US EPA method 1633, for biosolids, is included in Appendix A. This list will be updated periodically.
The sampling and analysis dates on the certificate of analysis must both be within the previous 6 months
Testing must be done using draft US EPA method 1633 (see section 6. Analytical method)
Results must report that the biosolids sampled have a concentration of PFOS below 50 ppb on a dry weight basis.
- Guidance for reading a certificate of analysis is included in Appendix B.

Attestation

For biosolids sold in Canada as fertilizers, an attestation document (Appendix D) must be completed in full, signed by the responsible party (producer or seller), maintained in records and provided to CFIA inspectors, upon request.
For biosolids imported into Canada as fertilizers, the attestation is embedded into AIRS, no separate document is required for import (do not use the document in Appendix D for import). However, if the imported product is subsequently sold in Canada, then an attestation document (Appendix D) is required, as for all other domestic sale, as described in the bullet above.

A product proponent can bring a product back into compliance by changing the manufacturing process and/or mixing clean, uncontaminated material with other inputs to effectively lower the concentration of PFOS in the source material. In any case where changes are made to manufacturing or processing, a new laboratory analysis is required.

5. Sampling and sample handling

Specific sampling requirements and sample handling considerations are detailed in Appendix C.

The intent of the sampling methodology is to ensure that the sample obtained is representative of the composition of the product, as it is imported or sold. As PFAS can be found in everyday products, special care must be taken to maintain sample integrity and avoid cross-contamination.

6. Analytical method

Draft United States Environmental Protection Agency's (US EPA) method 1633 (PDF): Analysis of per- and polyfluoroalkyl substances in aqueous, solid, biosolids, and tissue samples by LC-MS/MS is the single laboratory validated method that provides a standardized approach to measuring PFAS (including PFOS) in biosolids.

To demonstrate compliance with the interim standard, samples must be analysed by an accredited lab using draft US EPA method 1633. The acceptance of a single method is an interim approach that will change as additional validated methodologies become available.

All biosolids, including those with low solids content, should be analyzed as solids and reported on a dry weight basis.

7. Safety standards

In addition to meeting the PFAS standard, commercial biosolids (those that require registration and those that are exempt) must adhere to the prescribed standards as outlined in Trade memorandum T-4-93 – Safety standards for fertilizers and supplements with respect to the product's composition and contaminant levels.

8. Labelling requirements and registration application

General labelling requirements are outlined in Trade memorandum T-4-130 – Labeling requirements for fertilizers and supplements. For commercial biosolids requiring registration, guidance on submitting applications for product registration can be found in the Guide to submitting applications for registration under the Fertilizers Act.

9. Contact information

Fertilizer Safety Section
Canadian Food Inspection Agency
Phone: 1-855-212-7695
Email: cfia.paso-bpdpm.acia@inspection.gc.ca

Appendix A: Laboratories

This list will be updated periodically.

Analyses from any laboratory with the appropriate accreditation will be accepted.

The laboratory must be accredited by a body that is a signatory of the International Laboratory Accreditation Cooperation Mutual Recognition Arrangement (ILAC MRA) and have draft US EPA method 1633 (PDF) listed on their scope of accreditation for biosolids.

Laboratories known to be accredited for draft US EPA method 1633 for biosolids:

Appendix B: Certificate of analysis guidance

A descriptive overview of a certificate of analysis / laboratory report and an example results section from a sample certificate of analysis is provided in this appendix.

In general, a laboratory report will include:

a cover page
a list of abbreviations used
a summary of any sample analysis issues the laboratory may have encountered
a report of sample results including dates and times of sample collection and sample receipt
sample preparation and analysis details
laboratory quality control measurements, and
a copy of the chain of custody form for the sample.

The following table lists the common headings found on a certificate of analysis and provides explanatory text for each column. In this example, the result for PFOS is 6.3 ppb (or 6.3 ng per g), which is less than the limit of 50 ppb and therefore compliant with CFIA's interim PFAS standard. On an actual lab report, there will be a long list (40+) of analytes, this example includes PFOS only.

Sample results section of a certificate of analysis

Analyte	Result	Units	RL	MDL
Perfluorooctane Sulfonic Acid (PFOS)	6.3	ng/g (nanograms per gram)	1.7	0.14

Understanding each column

Results

The concentration detected.

This number is to be compared to the interim standard of 50 ppb to determine compliance.

Units

Common reporting units:

ng/g equals 1 ppb
ug/kg (micrograms per kilogram) equals 1 ppb
ng/kg (nanograms per kg) equals 1 ppt (parts per trillion)
1000 ppt equals 1 ppb

For a sample to be compliant with the interim standard, the result must be below (all are equal):

50 ppb
50 ng/g
50 ug/kg
50,000 ppt
50,000 ng/kg

Reporting limit (RL)

The limit to which the laboratory equipment can reliably report.

Method detection limit (MDL)

The lowest concentration that the laboratory test can detect a contaminant.

Appendix C: Sampling guidance

Specific sampling requirements for testing using US EPA method 1633 (PDF), the single required method for the CFIA's interim PFAS standard, are included below.

It is recommended to confirm sampling requirements with the contracted laboratory, prior to submitting samples for PFAS testing.

Requirements for sampling

Frequency

Sampling and testing is required (at minimum) every 6 months. Sampling twice a year is required to account for potential variation in inputs and treatments that may occur over the course of the year.

Sample containers

2 × 500 mL high-density polyethylene (HDPE) bottles with linerless HDPE or polypropylene caps.
Fill bottles no more than ¾ full, do not fill the bottle past the shoulder.

Collection method

There are 2 types of sample collection that may be utilized for biosolids, composite and grab. The conditions for choice of collection method are described here. In either case, the key is to obtain a representative sample of the product, as it is imported or sold.

Composite sample

When biosolids have been stored after the dewatering treatment processes, a composite sample should be obtained by collecting equal amounts of biosolids from multiple randomly selected locations and depths (minimum of 5 locations and 5 depths) and over larger areas, such as drying beds, various storage tanks or piles.

Grab sample

A grab sample should only be collected when biosolids are expected to be well mixed, for example when flowing past a sampling point. Each grab sample collected should be representative of the total solid stream flow passing the sampling point.

Packaging for shipment

Each sample bottle should be sealed individually in a Ziploc or Whirl–Pak® type bag.
Samples should be shipped to the laboratory in a cooler packed with double bagged wet ice or with sufficient frozen blue ice packs to maintain temperature below 6°C for 48 hours to account for any shipping delays.

Temperature and conditions

Samples must be protected from light from the time of collection until receipt at the laboratory.
Samples must be received by the laboratory below 6°C within 48 hours of sampling.

General precautions

Avoid eating food, using personal care products, sunscreen or insect repellant in the sampling area.
Powderless nitrile gloves should be worn and changed at any possibility for cross-contamination.
Ball-point pens or fine/ultra-fine Sharpie® markers are acceptable for labels. Regular/thick size markers (Sharpie® or otherwise) are to be avoided as they may contain PFAS.

Appendix D: Attestation document

The following document is required to be completed and maintained in records for biosolids fertilizers sold in Canada. This document is not required for importation as the attestation is written into the import process, however if the imported product is subsequently sold in Canada, the document is required.

Download the Attestation for sale of biosolids represented as fertilizers (PDF 157 kb)

Long description – Attestation form for sale of biosolids represented as fertilizers

Responsible part information (seller, producer, etc.)

Name:
Address:
Email:
Phone number:
Name of primary contact:

Attestation

I am aware of the requirements imposed by the CFIA's interim PFAS standard for biosolids represented as fertilizers, which are outlined in T-4-132: PFAS standard for commercial biosolids imported or sold in Canada as fertilizers.
- Yes
- No
The certificate of analysis accompanying this attestation is representative of the material being sold. I confirm that:
- the material was tested no more than 6 months prior to the date of sale.
  - Yes
  - No
- the link between the certificate of analysis and the biosolids batch is documented and can be verified.
  - Yes
  - No
- the sampling method, test methodology and lab accreditation all meet the requirements of the standard.
  - Yes
  - No
- the certificate shows PFOS concentration to be less than 50 parts per billion (ppb), on a dry weight basis.
  - Yes
  - No

Certificate of analysis associated with the batch/lot

Certificate of analysis number (or other identifier such as a work order number):
Date of issuance:

Declaration
I hereby declare that the information provided in this document is true and accurate. I am aware that providing false or misleading information to the CFIA is a contravention of Section 8(2) of the Fertilizers Act, and may create a risk of injury to human, plant and animal health, and the environment. I understand that I must maintain a copy of this attestation and of the certificate of analysis referenced above for review by the CFIA upon request.

Name of person who completed the attestation:
Business name:
Date: