The Method Update Rule-- 2017 - Mitchell Williams

The Method Update Rule-2017 Does this affect me? HOW? Method Updates Standard Methods updated to reflect those published in the 22nd Edition Method number with the year of

publication The method for BOD/CBOD is SM 5210 B-2011 Standard Methods Updated methods refer to quality control sections

1020Chemical and Radiochemical analyses 20202000 Methods (Turbidity, Acidity, Hardness, Solids, etc.) 3020 3000 (Metals) and 4000 (Inorganic Nonmetallic Methods 9020Microbiology

Micro Methods Some changes to SM 9222B (Standard Total Coliforms) Allows use of humidified incubator Added a note in Procedure section 4.5f that

at least 5 typical and atypical colonies must be verified per membrane The calculation of coliform density (Section 5b Water of other than drinking water quality) has been modified to be more like the EPA Microbiological counting rules Micro Methods... SM 9222D-2006 Thermotolerant (Fecal) coliform Membrane Filter Procedure

Footnote 30 was added to Table IA, requiring on a monthly basis, at least ten blue colonies from the medium must be verified using Lauryl Tryptose Broth and EC both Updated EPA Methods Pesticides

and PCBs: 608 is now 608.3 Includes additional analytes Allows for alternate detector; Requires confirmation of identification Added reporting limits Allows for SPE Allows for method modifications VOA and SVOA Organics

Volatiles--624 is now 624.1 Expanded scope to include additional analytes Allows for method modifications Allows for flexibility

Semivolatiles625 is now 625.1 Changes are very similar to those in 624.1 ASTM and USGS Methods Approval of new versions of currently approved ASTM Methods New USGS Methods for the Colorimetric

Determination of Nitrate Plus Nitrite in Water by Enzymatic Reduction, Automated Discrete Analyzer Method Approved ATPs IDEXX Laboratories, Inc., Colilert 18 for Fecal Coliforms in Wastewateraddition of increased incubation temperature for fecal coliforms, which requires the use of a water bath HACH 10242: Simplified Spectrophotometric Measurement of TKN in Water and Wastewater

HACH 10206: Spectrophotometric Measurement of Nitrate in Water and Wastewater Remember IDOPs! Corrections made to the 40CFR Typographical errors, technology updates, etc.

Whole Effluent Toxicity Acute and Chronic Methods Manualsclarifications in the definition of terms, consistency corrections among all three manuals. Table II, Required Containers, Preservation Techniques, and Holding Times Sodium thiosulfate concentrations for bacterial tests have been changed from 0.0008% to 0.008% sodium thiosulfate

Corrections/Clarifications Alternative Test Procedures Section: error in 2012 Method Update Rule appeared to give State permitting authorities the authority to approve ATPs for limited use. This was never the intent Only the Regional ATP Coordinator can

approve the limited use of ATPs Why a New MDL Determination Procedure? Addresses problems with the current procedure Blank contamination

Long-term variance Actual detectability Reduces false positives due to background contamination An option to have MDLs that represent multiple instruments MDL Determination Basics remain the same: MDL the lowest result that reliably indicates the analyte is in the sample

Calculation is unchanged The entire analytical process is incorporatedextraction, digestion How is it different? Definition has changed slightly... OLD--99% confidence that the analyte concentration is greater than zero... NEW99% confidence that the measured

concentration is distinguishable from method blank results... Inclusion of Method Blanks Low Level Spikes AND method blanks are analyzed over multiple days (at least 3) and multiple instruments An MDL calculated using the mean and standard deviation of MB results is compared with the MDL calculated from spiked samples

The greater MDL is used as the Reported MDL Initial Determination of MDL Blanks: Analyze at least 7 method blanks over a minimum of 3 days. Existing data is preferred; Calculate the MDLB using the formula: MDLB = mean +(SD)(Students t value) MB results must be numerical; may be POSITIVE

or NEGATIVE Use Zero for the mean if it is negative If all MB results are Non-detect (no peak on a chromatogram) the MDLB does not apply Spiked Samples... Prepared and analyzed over at least 3 calendar days Calculate the MDLS as per usual: MDLS = SD(Students t value)

Compare results The reported MDL will be the greater value MDLB or MDLS Ongoing Data Collection Only use data associated with valid calibrations and batch QC Analyze at least two spikes (in separate batches) on each instrument per quarter for a total of at least 7 per year. Spike at the same concentration as the initial MDL spikes

IF > 5% of the spikes are not positive numerical results that meet method identification criteria, increase spiking level and re-determine initial MDL Collection of MB Data Analyze

at least 7 blanks per year Use routine MB that are part of batch QC from the last 24 months If the number of MB>100, may use the 50 most recent results or those generated within the most recent 6 months whichever is greater Annual Verification of MDL Every 13 months using the collected

data from the past 24 months MB from the past 24 months Spiked samples at the same concentration as initial MDL spikes Include the initial MDL spikes if generated during the 24 month time frame Re-calculate the MDLB & MDLS

The verified MDL is the greater of the two values If the verified MDL is within 0.5 to 2.0 times the existing MDL, and fewer than 3% of the MB results have numerical results above the existing MDL, then the existing MDL may optionally be left unchanged. Otherwise, adjust the MDL to the new, verification MDL MDL Procedure

Implementation Issues Different process, new mind-set! Remembering to analyze quarterly spikes Keeping up with the data Possibly hundreds of method blank results to consider Multi-analyte tests such as volatiles, semivolatiles a bit cumbersome Learn the calculation rules When will the MUR be approved?

The MUR goes into effect 30 days after publishing date in Federal Register No estimated publication date! How long will I have to implement the changes? Begin addressing the changes immediately New methods such as 624.1, 625.1, and

608.3 take time to learn and implement To implement MDL guidelines will not be instantaneous The MUR of ???? Approval of updated methods Some old methods are going away608, 624, 625608.1, 624.1, 625.1 Approval of ATP methods: IDEXX for fecal; HACH 10242 for TKN; HACH 10206 for Nitrate

Need to perform an IDOC for any new methods The new procedure for MDL determination Questions? [email protected] For your attention!

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