EPA's Revision to the 40 CFR Part 136 Method Detection Limit (MDL) Procedure
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1 Ask The Expert Webinar Series EPA's Revision to the 40 CFR Part 136 Method Detection Limit (MDL) Procedure Richard Burrows, Ph.D. Corporate Technical Director
2 A Revision to the Method Detection Limit EPA finalized a revision to the 40 CFR Part 136 MDL procedure in the Federal Register on Tuesday August 8th This is a final rule with publication in the Federal Register expected mid-september 2
3 Presentation Summary Part 1 History of the MDL Part 2 What the MDL is Part 3 Problems with the MDL Part 4 Why we need a MDL Part 5 Details of the modifications Part 6 How the modifications improve the procedure Part 7 What does this mean to labs and data users?
4 History of the MDL
5
6 Further developments 1984 USEPA the MDL procedure is promulgated in 40 CFR, Part 136, Appendix B for use in the wastewater program and defined as 3.14 times the standard deviation of seven low level spiked blanks. The ML is also promulgated at this time The MDL is widely adopted by other programs within EPA and written into many state and federal regulations USEPA published Method 1631B for analysis of mercury using the old MDL approach and modified ML definition, which provided an opportunity for a legal challenge of the MDL and ML USEPA entered into a settlement agreement with the Alliance of Automobile Manufactures, Chemical Manufacturer s Association, Utility Water Act Group and AFPA.
7 Further Developments 2002 USEPA issues a Technical Support Document of Detection and Quantitation Regulations under the Clean Water Act (TSD) Draft revised MDL published 2003 Consensus letter submitted to Assistant Administrator of Office of Water signed by 31 parties urging EPA to consider a scientifically sound approach to the detection and quantification issue.
8 Yet More 2005 Federal Advisory Committee on Detection and Quantification (FACDQ) formed by USEPA Office of Water as a result of the 2000 Settlement Agreement 2007 FACDQ completes their work issuing a final report with recommendations, with Office of Water to complete a post FACDQ pilot study based on FACDQ recommendations.
9 And even more TNI forms Environmental Methods Measurement Expert Committee based on a USEPA grant to address Calibration, Detection, Quantification and other measurement issues Final report on Post FACDQ pilot study issued, recommending further evaluation with additional methods and analytes TNI EMEC (renamed Chemistry committee) completes work on a MDL revision and submits to EPA 2014 EPA completes internal review of the revised MDL and makes minor modifications 2015 EPA publishes revised MDL as part of a Methods Update Rule 2017 Signed by EPA Administrator Scott Pruitt
10 What is the MDL?
11 Lloyd Currie s original concept L C The lowest result that can be reliably distinguished from a blank Equals the MDL equals the TNI LOD L D The lowest amount present in a sample that will reliably give a result that is above L C Not routinely used in environmental testing (included in the DOD QAPP) L Q The lowest amount that gives quantitative results Conceptually, equals TNI LOQ, EPA ML and EPA LLOQ
12 MDL MDL The method detection limit (MDL) is defined as the minimum measured concentration of a substance that can be reported with 99% confidence that the measured concentration is distinguishable from method blank results MDL 3.14 x Standard Deviation 0 MDL 40 CFR Part L C Currie s Critical Level
13 What the MDL is (and is not): MDL = Lowest result that can be distinguished from blanks Or, lowest result that means there is actually something in the sample MDL Lowest amount in a sample that can be reliably detected
14 MDL and Currie s L D Currie s L D is the minimum true concentration that is reliably detected (i.e., gives a result above the MDL) MDL L D 1% chance of false negative 0 MDL CFR Part L C L D Currie s Detection Level 0 DL (LODDOD) DOD
15 What does this mean regarding verification? MDL can be verified by examining blank results MDL cannot be verified with spiked samples (Curries L D could be verified with spiked samples)
16 Problems with the Current MDL
17 Blank bias Current MDL assumes blank results are centered around zero If blanks are not centered around zero, then the MDL will be too low and many false positives will result MDL 3.14 x Standard Deviation of 7 spikes 0 MDL 40 CFR Part L C Currie s Critical Level
18 Lead in Particulate Matter 350 Ultrasonic extraction Quartz filter blanks Blank result MDL(S) X+ts
19 Variance and Verification Current MDL assumes that short term and long term variance are the same Variability of instrument response in one batch is the same as variability of instrument response over the course of a year??? Current MDL has no verification that results obtained are reasonable
20 Why Do we need a MDL?
21 Reason #1 that we need MDLs We need to make the Quantitation limit meaningful Applies to MRL, LLOQ, or any quantitation limit
22 Reported Concentration 90% recovery, 9% RSD Spike #1 #2 #3 #4 #5 #6 #7 Mean MDL Spike True Value = LLOQ Mean recovery MDL = 2.29 Calculated MDL Replicate Number Reported results (without MDL) ND ND ND ND ND ND 10
23 If you run 100 spikes at LLOQ What if you have 70% average recovery? Assume 10% RSD Now 99% False Negative Rate ZERO MDL LOQ
24 Reason #2 that we need MDLs MDLs are needed in risk assessment Handling non-detects ~ Substitute a value such as ½ detection limit or detection limit ~ More sophisticated methods such as Maximum Likelihood estimation and Regression on Order statistics These still benefit from a detection limit as low as possible If we do not have a detection limit, the Quantitation limit will become the new Detection limit
25 Details of the Modifications
26 First, what stays the same? Fundamental concept is unchanged What is the lowest result that is qualitatively reliable, i.e., the lowest result that reliably indicates the analyte is in the sample? Fundamental approach is unchanged Describe the distribution as Student s t times the standard deviation of results
27 Revised MDL Procedure Flow Chart INITIAL DETERMINATION OF MDL Run 7 low level spikes Run 7 method blanks Fix problem or raise spike level and repeat No Do results meet qual ID? Yes Calculate MDLs Calculate MDLb Set higher of MDLs and MDLb as MDL
28 Spikes and Blanks INITIAL DETERMINATION OF MDL Run 7 low level spikes Run 7 method blanks Fix problem or raise spike level and repeat No Do results meet qual ID? Yes Calculate MDLs Calculate MDLb Set higher of MDLs and MDLb as MDL
29 Qualitative identification INITIAL DETERMINATION OF MDL Run 7 low level spikes Run 7 method blanks Fix problem or raise spike level and repeat No Do results meet qual ID? Yes Calculate MDLs Calculate MDLb Set higher of MDLs and MDLb as MDL
30 Qualitative identification INITIAL DETERMINATION OF MDL Run 7 low level spikes Run 7 method blanks Fix problem or raise spike level and repeat No Do results meet qual ID? Yes Calculate MDLs Calculate MDLb Set higher of MDLs and MDLb as MDL MDL S = Students t x Standard Deviation of the spikes MDL B = Mean of blanks + Students t x Standard Deviation of the Blanks
31 Compare MDL S and MDL B INITIAL DETERMINATION OF MDL Run 7 low level spikes Run 7 method blanks Fix problem or raise spike level and repeat No Do results meet qual ID? Yes Calculate MDLs Calculate MDLb Set higher of MDLs and MDLb as MDL
32 Details, details Spiking level 2-10 times estimated MDL Run spiked replicates in at least 3 separate preparation and analysis batches Multiple instruments At least 2 spike replicates on each instrument If blanks give ND, MDL B does not apply Addendum for MDL determined on a specific matrix No 10X rule Use all method blanks unless batch was rejected
33 Does the 10X rule protect against MDLs that are too low? True Results within =/- 3% Mean RSD Std Dev MDL % True Results within =/- 40% Mean RSD Std Dev MDL %
34 Ongoing verification
35 Quarterly date collection / verification Analyze at least one spike on each instrument (2 if only one instrument) Correct problem and repeat or repeat initial at higher concentration No Do results meet qualitative ID? Yes No actions needed 36
36 Annual recalculation Collect Spike Data and Recalculate MDL S Collect Blank Data and Recalculate MDL B Is the newly calculated MDL within 3X of the existing MDL? NO YES Change MDL to the newly calculated MDL Option: Leave the MDL unchanged or change to the newly calculated MDL 37
37 How the modifications improve the procedure Sensible MDLs when there is blank bias 1980 Lead in tuna results overstated by 1000X due to blank contamination 2004 EPA Episode 6000 data Chromium by ICPMS, 1400% recovery at the MDL and 600% recovery at the ML due to blank bias 2013 Multi-lab blank detection rates ~ 8270 SIM 6.4% ~ 8921B 16% ~ ICPMS 8% 2014 Lead in particulate matter ~ All blanks in the validation study exceeded the MDL This problem is getting worse because of the need for low level data and increasing sensitivity of instrumentation
38 How the modifications improve the procedure Long term vs. short term bias The difference varies from method to method and lab to lab, but can be large Long term bias is what matters when it comes to the MDL Ongoing verification Very consistent with EPA office of Water MRL, EPA ORCR LLOQ and the proposed TNI LOQ
39 What does this mean to labs? Clear requirements Sensible MDLs Level playing field Low transition costs since existing data can be used Note labs should start complying with 3 batch rule right now Some additional organizational requirements
40 What does this mean to data users? MDLs that make sense Much lower rate of false positives, especially for ICP, ICPMS and some general chemistry tests Easier to compare labs In general, more reliable data = better decision making
41 How much will MDLs change? Analytes with minimal or no detects in blanks, eg most GC/MS analytes at normal levels: Not Much Analytes with frequent detects in blanks, eg, metals, very low level PAH, some general chemistry tests: Depends If the lab is currently adjusting MDLs to avoid excessive false positives, not much If the lab has been pushing MDLs below levels justified by the blanks, potentially quite a bit
42 How can YOU help? (Google EPA 2015 Methods Update Rule) Submit your comments, identified by Docket ID No. EPA HQ OW , by one of the following methods: Follow the on-line instructions for submitting comments. Attention Docket ID number EPA HQ OW WE ENCORAGE EPA TO ADOPT THE CHANGES TO THE 40 CFR PART 136 APPENDIX B MDL PROCEDURE IN FULL
43 Ask The Expert Webinar Series Thank you for attending EPA S Revision To The 40 CFR Part 136 Method Detection Limit (MDL) Procedure To submit a question, type it into the Questions panel in the GoToWebinar toolbar and click Send. If you have any additional questions for today s presenter you may submit them directly to: Please be sure to visit the Ask the Expert Webinar Series web page for other scheduled webinars at: To view a recording of this webinar session, please contact: info@testamericawebinars.com
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