1. Overview CWA Methods Update Rule Method 608.3
August 2017 • Adrian Hanley, U.S. EPA

2. Methods Update Rule (MUR)
CWA MUR every 3-5 years
Previous CWA MUR finalized in 2012
Current CWA MUR
Proposed February 19, 2015
175 sets of comments received
OMB Found the rule not significant under Executive Order on April 13, 2016
Originally signed on December 15, 2016
Withdrawn from the FR, being reconsidered
Not significant means neither financially significant nor controversial

3. Action Development Process for the MUR
Rule proposed and comments received
Respond to comments
Modifications for final rule may occur
Internal Review of Final Rule
Multi-office EPA workgroup including Office of General Counsel and Office of Policy
Rule finalized, signed by Administrator
Becomes effective upon publication
Important Note: When finalizing a rule, items from the proposed rule are generally accepted, rejected, or modified. New items outside of the scope of the proposed rule are generally not added to the final rule.
Followed the Action Development Process (ADP).

4. Methods 608.3, 624.1, and 625.1
Pesticides and PCBs, volatile and semivolatile organic compounds
Revision – made limited changes:
Updated technology
Capillary columns, updated references
Method Flexibility
Allows more changes with internal documentation (no ATP required)
Follow 40 CFR Part 136.6
Method Harmonization
Enhances consistency among EPA method programs: drinking water, solid-waste, superfund
Three revised EPA Methods: 624 and 625 (volatile and semivolatile organic compounds) and 608 (Pesticides and PCBs)
Have not been revised since promulgation in 1984
Laboratory stakeholders asked for a long overdue revision of these methods.
Revisions reflect collaboration with other EPA program offices, EPA regions, technology vendors, states, and laboratory organizations in a multi-year process via workgroup before proposal
Revisions incorporate:
Technology updates that have occurred in the more than thirty years since these were originally promulgated Harmonization with similar methods in other EPA offices (e.g., frequency of QC testing, calibration criteria, etc…) in order to reduce the workload at laboratories that run methods for multiple EPA programs
Primary comments: (1) Comments in support of the overall revisions, (2) Many highly varied comments regarding minor technical details – some resulted in minor revisions, (3) Many requests to tighten published QC limits and lower published detection limits, which would require a multi-laboratory study

5. Method 608 to 608.3 Underwent 2 rounds of review before proposal
EPA Regions then select reviewers
Proposed Rule in 2015
Received 210 pages of tabulated comments
Resulted in many minor revisions
Current Version of 608.3
Pre-publication available at:

6. Disclaimer
The following slides are only a summary of the changes made from Method 608 to Method The slides do not contain every single change, just the changes that this presenter believes are most significant.

7. Additional Analytes Table 2: Additional Analytes
New analytes not approved under 40 CFR part 136
Intended for analytes of interest (see 1.4)
Cost savings for dischargers
Initial Demonstration of Capability required
Default MS/MSD recovery of % and RPD of 30%, unless tighter in house criteria are available (see )
Aroclors and Toxaphene
Moved to Table 2
Not required for QC tests (see 1.5)
1.4 The large number of analytes in Tables 1 and 2 makes testing difficult if all analytes are determined simultaneously. Therefore, it is necessary to determine and perform quality control (QC) tests for the “analytes of interest” only. The analytes of interest are those required to be determined by a regulatory/control authority or in a permit, or by a client. If a list of analytes is not specified, the analytes in Table 1 must be determined, at a minimum, and QC testing must be performed for these analytes. The analytes in Table 1 and some of the analytes in Table 2 have been identified as Toxic Pollutants (40 CFR ), expanded to a list of Priority Pollutants (40 CFR part 423, appendix A).
1.5 … Toxaphene and the PCBs have been moved from Table 1 to Table 2 (Additional Analytes) to distinguish these analytes from the analytes required in quality control tests (Table 1). QC acceptance criteria for Toxaphene and the PCBs have been retained in Table 4 and may continue to be applied if desired, or if these analytes are requested or required by a regulatory/control authority or in a permit. …

8. Calibration
Recommend 5 standards for single component analytes (minimum of 3 standards)
Calibration curve can be used
Consistent with 40 CFR part 136.6
6 standards are required for curve fits and relative standard error calculations
Aroclors
Minimum of 3 standards containing both Aroclor 1016 and 1260
Single midpoint standards of the other 5 Aroclors
Toxaphene
Minimum of 3 standards

9. QC Changes Can repeat failed QC tests for failed analytes
Only when many analytes are analyzed, and 80% of the analytes pass
No maintenance or adjustments in between
Calibration Verification Standards (see 6.8.4)
Prepared using standards obtained from a second source
Note: Second source standards are optional for MS/MSD and LCS samples (see 6.8.3)

10. QC Changes (cont.) Surrogates are required
Examples: dibutyl chlorendate (DBC), tetrachloro-m-xylene (TCMX), 4,4'-dibromobiphenyl, or decachlorobiphenyl
Alternative surrogates and concentrations allowed
Blanks are reported to the MDL
GC resolution criteria added (see 13.4)
Valley height 40% of the shorter peak
DDT and Endrin decomposition criteria added
Breakdown <20% (see 13.5)

11. Extraction/Cleanup
Additional procedures for continuous liquid-liquid extraction (CLLE) and disk based solid phase extraction (SPE)
CLLE is essentially an automated liquid-liquid extraction, which is allowed under 40 CFR part 136.6
Disk based SPE is based on an approved alternate test procedure
(60 FR 39585, August 2, 1995)
More cleanup procedures are provided
Always have been allowed under method flexibility
Contained within “Solutions to Analytical Chemistry Problems with Clean Water Act Methods”

12. New Allowed Modifications
New materials can be vendor certified by one laboratory (see )
Most relevant to solid phase extraction
Requires an Initial Demonstration of Capability
Requires testing in specified 9 matrix types (see )
Must meet Table 4 MS/MSD criteria
Default criteria if no Table 4 data available
60 to 140% recovery and 30% RPD
Full data packages must be made available, and kept by the laboratories using the new materials (see )

13. Common Comments
Remove 5% MS/MSD frequency requirement for each discharge site
Not a significant change, 608 requires 10% frequency
Reviewed and approved by the Science Advisory Board during original promulgation in 1984
Proposed MDLs are invalid
MDL were changed back to original values
Do not reference unapproved methods
Only referenced in the context of analytical trouble shooting

14. Common Comments (cont.)
Require 5 calibration standards
Change “Fill in the blank” criteria
Need a multi-lab validation
Criteria were taken from a different EPA method program, so it is fostering method harmonization
EPA should not allow reporting to the MDL
That is the decision of the permitting authority

15. For more information or additional feedback, please contact:
Contact Information
For more information or additional feedback, please contact:
Adrian Hanley, US EPA Office of Water
Office of Science and Technology Phone:
Does anyone have any questions, comments, or feedback?
If you have additional comments or would like to provide feedback on the issues raised in this presentation, please feel free to contact me.