Method Update Rule (MUR) impact on Detection Limits
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1 Method Update Rule (MUR) impact on Detection Limits David Gratson, CEAC Lester Dupes, CEAC Jennifer Gable Amanda Cover 4C Conference, April, 2018 San Antonio, TX 1/9/18 Page 1
2 Agenda Method Update Rule (MUR) Background Blanks and Reporting under MUR MUR definitions for MDL Impact on MDLs old/new MAL = ML? Questions 1/9/18 Page 2
3 MUR a bit of history Clean Water Act (CWA) Methods 40 CFR Part 136 General Purpose and Industry Specific Effluent Guidelines NPDES Discharges E.g., Petroleum Refining, Pharmaceutical Industry Study MUR used to update analytical methods required under the CWA Updates 2003 (microbial methods for ambient water) 2007 (microbial methods for wastewater and sewage sludge) 2012 (pesticides, new purgeable analytes, O&G) 2017 Alternative Test Procedures under 40 CFR Part 136 1/9/18 Page 3
4 2017 MUR These revisions: provide increased flexibility to the regulated community improve data quality update the methods, to keep current with technology advances address laboratory contamination issues related to the MDL and better account for intra-laboratory variability. 1/9/18 Page 4
5 2017 MUR Update to EPA methods, Standard Methods, ASTM and other methods Changes to sample preservation and holding times for microbiology Revised MDL Procedure Other Technical Corrections 1/9/18 Page 5
6 2017 MUR MDLs and Minimum Limits (ML, aka reporting limits) provided in the methods for most analytes Laboratories: MDLs are to be equal or lower than published OR 1/3 compliance limit Theory ML = 3.18 * MDL (L Q *), MUR uses just 3X Significant Figures Method Table - Endosulfan sulfate MDL = 66, ML = 198 * Lloyde Currie (1968, limit of quantification) 1/9/18 Page 6
7 2017 MUR Blanks One blank per batch Re-extract if blank result is: Greater than MDL, or Greater than 1/3 compliance limit, or Greater than 1/10 sample concentration 1/9/18 Page 7
8 2017 MUR Reporting (NPDES) Report Native Sample Results to ML (not MDL) 3 significant figures Report Blanks Results to MDL 2 significant figures Allow for blank subtraction if requested or required by method 1/9/18 Page 8
9 Method Detection Limit (MDL) a bit of history 1984 The current procedure for calculating the MDL was promulgated in 40 CFR 136, Appendix B Measuring seven low level spiked blanks and multiplying the standard deviation 3.14 to determine the MDL. Minimum Level (ML) also defined at this time 1999 US EPA published Method 1631B for analysis of mercury using the 1984 MDL approach and modified the ML 2000 US EPA entered into a settlement agreement 1/9/18 Page 9
10 Method Detection Limit (MDL) Assumptions Blank results are centered around zero. Not always true, thus has a high potential for underestimating the MDL, resulting in false positives. Short term variance = is the same as long term variance. It therefore has a high potential for underestimating the MDL, resulting in false positives Homoscedasticity 1/9/18 Page 10
11 MUR Revision Variance Must include at least three batches on three separate calendar dates Must include multiple instruments over multiple days Both approaches more realistic variance Can expect fewer false positives 1/9/18 Page 11
12 1/9/18 Page 12
13 MDL Algorithms MDL S All analyses must meet qualitative criteria. MDL s = t n 1,1 α 0.99 s s 1/9/18 Page 13
14 MDL Algorithms MDL b Results If no numeric results (+ or -), MDL = MDL s If ALL numeric results (+ or -), MDL b = തX + t n 1,1 α 0.99 s b where t = Students t for n-1. If SOME numeric results (+ or -): If 100 results, MDL B = highest blank result If >100 results: MDL b = n 0.99 th rounded ranked MB result 1/9/18 Page 14
15 MUR Revision This will be particularly significant for results from: inductively coupled plasma (ICP)/AES ICP/mass spectrometry (MS) many wet chemical parameters, where blank results are uncensored. Censored blank results (GC, GC/MS) Might these produce the same MDL as the current procedure, propagating the issue of artificially low MDLs? 1/9/18 Page 15
16 Censoring Censored blank results (GC, GC/MS) Software algorithm evaluates chromatogram for level above which area used to estimate concentration, below = censored Might these produce the same MDL as the current procedure, propagating the issue of artificially low MDLs? 1/9/18 Page 16
17 Element % D 6020 Water Element % D 6020 Water Ag 55% Mn 110% Al 65% Mo -38% As 60% Na 36% B 172% Ni -42% Ba 135% Pb 130% Be 24% Sb 19% Ca 56% Se 114% Cd -64% Si 80% Co 125% SiO2 86% Cr 11% Sn 67% Cu 78% Sr 151% Fe 80% Ti 79% K 47% Tl 38% Li 92% V 51% Mg 99% Zn 17% %D = difference average 1/9/18 Page 17
18 Element % D 6020 Soil Element % D 6020 Soil Ag 47% Mn 132% Al 104% Mo 40% As 34% Na 90% B 122% Ni -28% Ba 105% Pb 136% Be 106% Sb 12% Ca 96% Se 93% Cd -21% Si 144% Co 107% Sn 50% Cr 44% Sr 150% Cu 80% Ti 1% Fe 80% Tl 40% K 17% V -21% Li 92% Zn 39% Mg 153% P 54% %D = difference average 1/9/18 Page 18
19 Element % D Water Element % D Water Ag -23% Mn 138% Al 66% Mo -43% As 107% Na 89% B * 101% Ni -30% Ba 16% Pb 134% Be 83% Sb -48% Ca 95% Se 59% Cd -81% Si 58% Co 104% Sn -12% Cr 26% Sr 128% Cu 56% Ti 26% Fe 75% Tl 4% K -11% V 60% Li 35% Zn -7% Mg 102% %D = difference average 1/9/18 Page 19
20 TCEQ MAL = MLs? Some MLs and MDLs in the rule are lower than those in TCEQ s current Implementation Procedures for the Texas Surface Water Quality Standards (IPs), June 2010, RG-194, however some are higher. 1/9/18 Page 20
21 Thank You for your Time! Headquarters 1140 Valley Forge Road PO Box 810 Valley Forge, PA Virginia 1412 Sachem Place, Suite 100 Charlottesville, VA Tennessee 8331 East Walker Springs Lane, Suite 402 Knoxville, TN New Mexico PO Box Santa Fe, NM Illinois PO Box 335 Geneva, IL South Carolina PO Box Charleston, SC New Jersey 1175 Marlkress Rd. #4222 Cherry Hill, NJ West Virginia 2501 Chapline St. PO Box 6562 Wheeling, WV Web 1/9/18 Page 21
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