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Limit of Detection Guidance Document

Limit of Detection Guidance Document

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ANALYTICAL DETECTION LIMIT GUIDANCE& Laboratory Guide for Determining Method Detection LimitsWisconsin Department of Natural ResourcesLaboratory Certification ProgramApril 1996
PUBL-TS-056-96
 
introduction and background 
The Department of Natural Resources (DNR) formed a Technical Advisory Committee in November, 1990 atthe request of the Secretary of the Department to examine the LOD/LOQ language in Ch. NR 106, Wis. Adm.Code, and the corresponding language in WPDES permits to determine if the permit language was consistentwith the code, and if not, to formulate recommendations to achieve consistency. The committee's report (WIDNR, 1994), issued on January 2, 1994, recommended implementing new, consistent permit language basedupon scientific limitations. The report also addressed related LOD/LOQ issues facing the Department raisedthrough the investigation but not directly within the Committee's charge. These issues were deemed criticallyrelated to the LOD/LOQ issue and the Committee urged the Department "to give serious consideration toimplementing (these) recommendations". Among them:1.The Department needs to provide permittees with guidance instructing them how to report, interpretand apply sampling results that are below the LOQ.2.The Department needs to develop uniform definitions of LOD and LOQ which are applicable to allenvironmental sampling programs.The need for consistent definitions and low level data reporting across all of the agency's environmentalprograms compelled the Laboratory Certification Program, to play a significant role in coordinating theDepartment's efforts. The Laboratory Certification Code, Ch. NR 149, Wis. Adm. Code, which requireslaboratories to statistically determine their detection limits, was revised to address the Committees'recommendations. An amendment requiring laboratories to report analytical data for selected substances downto their calculated detection limit becomes effective January 1, 1997. This requirement was created tosupplement other Administrative Codes, many of which already require facilities and site owners to reportanalytical data down to a calculated detection limit. This rule change also modified the definitions of the limitof detection and limit of quantitation for consistency with Chs. NR 106, NR 140, proposed NR 507, and NR809. Wis. Adm. Code.At the present time, the Department requires certified and registered laboratories to calculate detection limitsusing the U.S. Environmental Protection Agency Method Detection Limit (MDL) procedure found in Title 40Code of Federal Regulations Part 136 (40 CFR 136, Appendix B, revision 1.11). This method has both criticsand supporters. Despite its limitations, it remains the most widely documented and one of the simplest waysto calculate a detection limit. However, the procedure is often misunderstood, and invalid MDLdeterminations are common. The Department conducted an interlaboratory survey of semivolatile organiccompounds detection limits in April of 1993. Of the 56 labs surveyed, 23 incorrectly calculated their MDLs.The Laboratory Certification Program developed this guidance to assist laboratories follow the procedurecorrectly and generate meaningful detection limits. These meaningful detection limits are a critical first steptoward meeting the agency's data needs of the future, where toxicology is expected to continue to push theboundaries of analytical science.This document interprets the Laboratory Certification Program's policy on limits of detection, and containshelpful hints and suggestions to assist laboratories calculate method detection limits. It provides alternativesfor analytical methods which do not lend themselves well to statistical detection limit determinations.Moreover, this document provides guidance for performing a "common sense check" on a calculated MDL.This document supplements the Code of Federal Regulations procedure for calculating the method detectionlimit. In all cases, the Federal Regulations protocol must be followed for calculating MDLs.
This guidance was written and edited by Jeffrey Ripp, a chemist in the Wisconsin Department of Natural Resources'  Laboratory Certification Program. Additional copies may be requested by writing to the Laboratory CertificationProgram, Wisconsin Department of Natural Resources, 101 S. Webster St., Box 7921, Madison, WI 53707. Or, visit theWisconsin DNR online at {http://www.dnr.state.wi.us}.
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Table of Contents
Part I. Definitions............................................ 1Part II. Method Detection Limits.................................. 32.1 What are Method Detection Limits (MDLs)?................... 32.2 Why do we need MDLs?................................. 42.3 Discussion of the MDLs' Limitations......................... 5Part III. Calculating Method Detection Limits......................... 63.1 Practical Considerations for Improving the MDL Procedure......... 63.1.1 Analytical Systems............................... 63.1.2 Calibrating for the MDL Procedure.................... 63.1.3 Choosing the Proper Spike Level...................... 73.1.4 Replicate Sample Preparation........................ 73.1.5 Analyzing Blanks................................ 83.1.6 Accounting for Day to Day Variability.................. 83.2 Calculations.......................................... 83.3 Frequency of MDL Determinations.......................... 93.4 Calculating MDLs for Multiple Instruments and Analysts........... 93.4.1 The 50% Rule................................... 93.4.2 The F-Ratio Test................................ 103.4.3 The Upper Critical Limit Test....................... 103.4.4 Screening Instruments............................ 103.4.5 Safe Drinking Water Instruments..................... 113.4.6 Examples of Multiple Instruments.................... 11Part IV. Validating MDL Determinations........................... 114.1 Common Sense Check.................................. 114.2 The Five Point Check.................................. 124.2.1 Meeting Requirements............................ 124.2.2 The S/N Test.................................. 124.2.3 Percent Recoveries............................... 134.3 Serial Dilutions...................................... 144.4 Iterative Procedure.................................... 14Part V. Examples and Special Cases.............................. 145.1 Ammonia by Ion Selective Electrode (ISE).................... 145.2 Atrazine by Gas Chromatography .......................... 155.3 Lead in Drinking Water by Graphite Furnace (GFAA)............ 165.4 Gasoline Range Organics (GRO) by the Wisconsin Method ........ 175.5 Common Wastewater Tests and Exempt Analytes............... 18
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