Enforcement of the interim standard at import and domestic levels will begin October 18, 2024. This allows four months from the publication of this trade memorandum for importers and domestic producers of commercial biosolids to arrange for a laboratory to perform the testing and have the certificate of analysis and attestation prepared in advance of the October enforcement start-date.
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 (Sewage sludge) and 38.25.10 (Municipal Waste)
- 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 (importer, seller or producer) is required to maintain a valid certificate of analysis and attestation 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
- The attestation form must be completed in full and signed by the responsible party (importer, producer or seller). The attestation form will be available here prior to the enforcement start date.
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: Analysis of per- and polyfluoroalkyl substances in aqueous, solid, biosolids, and tissue samples by LC-MS/MS (PDF) 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:
- A & B Environmental Services (USA)
- Alpha Analytical (USA)
- ALS Environmental (USA)
- American Analytics (USA)
- APPL (Metiri Group) (USA)
- Babcock Laboratories (USA)
- Battelle (USA)
- Bureau Veritas Canada (Canada)
- Enthalpy Analytical (USA)
- Eurofins (USA)
- GEL Laboratories (USA)
- McCampbell Analytical (USA)
- Merit Laboratories, Inc. (USA)
- Pace Analytical (USA)
- SGS AXYS Analytical Services (Canada)
- SGS North America (USA)
- Sterling Labs (USA)
- Suburban Testing Labs (USA)
- Symbio Laboratories US (USA)
- Torrent Laboratory (USA)
- Weck Laboratories (USA)
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.