The 2016 TNI Standards Presented by Zonetta E

The 2016 TNI Standards Presented by: Zonetta E. English, MBA On behalf of Jerry Parr, Executive Director, TNI

Current Status of 2016 TNI Laboratory Standard Volume 1: Laboratory Requirements Module 1: Proficiency Testing - FINAL Module 2: Quality Systems - FINAL Module 3: Asbestos – FINAL Module 4: Chemistry - FINAL Module 5: Microbiology - FINAL Module 6: Radiochemistry - FINAL Module 7: Whole Effluent Toxicity – No Changes

Other 2016 TNI Standards Volume 2: AB Requirements Volume 3: PT Provider Requirements Module 1: Accreditation Body – No Change Module 2: Proficiency Testing - FINAL Module 3: On-Site Assessment – No Change FINAL Volume 4: PTPA Requirements FINAL

2016 TNI Laboratory Standards See presentations made on Wednesday, July 1, 2015 at the 2015 NEMC http: //nemc. us/meeting/2015/techprog. php Click on the Wednesday tab! Updated versions of these presentations with more detail were made on August 11 at the 2016 TNI meeting Webinars likely this fall

2016 PT Standards Volume 1, Module 1 Reverse some decisions made in 2009 LOQ reporting Analysis date New sections for WET and Protozoa Radiochemistry now included Volumes 2, 3, and 4 Many changes affecting PT Providers Clarification of role of AB in reviewing PT results

Changes in Reporting TNI has published Proficiency Test Reporting Limits (PTRL) for every analyte: PTRLs are the lowest possible concentration of the analyte in the sample Lab LOQ must be equal to or greater than the TNI PTRL Results above LOQ should be reported without qualifiers If the Lab LOQ > PTRL, and the analyte is present, the result will be scored unacceptable See Note in Section 4. 3. 7 V 1 M 1

V 1 M 1 Study Date q Opening date of second study at least 7 days after the closing date of first study. q q No longer analysis dates This reduces the waiting time for a laboratory to analyze a second PT to have accreditation reinstated V 1 M 1

Whole Effluent Toxicity PTs q Whole Effluent Toxicity Allow the use of DMR-QA to meet PT requirements. Sets the frequency for WET to one time per year. Defines what the corrective action is to be submitted. V 1 M 1

Radiochemistry PTs Requirements same as Chemistry Analyze 2 PT samples per year Pass two of most recent three Analytes and Acceptance limits in Fo. PT tables Drinking water only V 1 M 1

V 1 M 2 Quality Systems Revised to include all of ISO/IEC 17025 verbatim q q Revised definition for Limit of Detection Revise temperature calibration (5. 5. 13. 1) Removed Note from Section 5. 6 on traceability Added back language in Sections 5. 4 on method validation Allow single point verification at mandated condition Other minor clarifications and revised definitions

Clarifications and Definitions q q “Parameter” was changed to “Analyte” Any Notes were either eliminated or had the “NOTE” removed – this makes them requirements Definitions Analyte (revised) Data Integrity (revised) Lot (added) Parameter (deleted) Physical parameter (added) Reference Method (revised) V 1 M 2

Reference Method A published method issued by an organization generally recognized as competent to do so. (When the ISO language refers to a “standard method”, that term is equivalent to reference method). Definition important for Module 3 -7, especially Module 4, Chemical Testing V 1 M 2

V 1 M 4 Chemistry Standard Revised Method Selection and Validation Revised Calibration Section Revised Section on LOD and LOQ Moved general language on method selection and validation to Module 2 V 1 M 4

1. 4 METHOD SELECTION When adding a new analyte to a reference method, the inclusion of the analyte in the method shall meet all required calibration requirements and the QC requirements of the method to which the analyte is being added. If no QC exists in the method, the laboratory shall adhere to the requirements outlined in a reference method of the same technology (when available). V 1 M 4 i. e. , Reference Methods do not need to be “validated” for new analytes

QC REQUIREMENTS 624 ICAL RSD: 35% CCAL: MIN RF: BFB Recovery: V 1 M 4 8260 ICAL RSD: 30% CCAL: 20% MIN RF: 0. 1 BFB Recovery: 86 -118

Instrument Calibration 2009 1. 7. 1 Initial Calibration 1. 7. 1. 1 Instrument Calibration 2016 10 subsections 1. 7. 1. 2 Continuing Calibration V 1 M 4 5 subsections 1. 7. 1 Calibration 1. 7. 1. 1 Initial Calibration 13 subsections 1. 7. 1. 2 Continuing Calibration Verification 6 subsections

Revised Calibration Section Removal of calibration points Number of standards required Relative Error / Relative Standard Error Corrective action for CCV Many other minor changes V 1 M 4

1. 7. 1 Calibration Clarifies that calibration of support equipment is in Module 2 Continues to allow other options in mandated methods or programs to supersede these requirements Clarifies that calibration may be performed at the instrument or method level V 1 M 4

1. 7. 1. 1 Initial Calibration Clarifies that results from most recent initial are to be used New section on removal and/or replacement of calibration standards Section on number of calibration standard completely revised New section on relative error New sections on Arochlors, sensitivity checks and upper reporting limits Other minor clarifications V 1 M 4

Anscombe’s Quartet

1. 7. 1. 2 Continuing Calibration Verification New section requires CCV to be < ½ high point Allows use a second source CCV Allows LCS to be used as CCV in limited cases Allows a second CCV to be used with justification V 1 M 4

Changes to LOD New definition for the LOD (in Module 2) Equivalent to EPA MDL Added several new requirements Samples used to determine LOD must be prepped analyzed over several days Evaluation of routine method blanks must be included ª Where appropriate use MDLB instead of MDLS Specifications for ongoing verification of LOD Made consistent with revised Method Detection Limit in 40 CFR Part 136 V 1 M 2

Changes to LOQ Minimum of 7 spikes at or below LOQ Details requirements if multiple instruments will have same LOQ is the spiking level, unless < 3 X LOD in which case LOQ is 3 X LOD Allows determination of precision and bias at the LOQ verification used for LOD determination V 1 M 4 One set of analyses; two results

V 1 M 5 Microbiology q Significant Rewrite for Clarity q q Clarified definition of source water Revised Method Selection and Validation Revised chlorine residual check Additional guidance and options Reinforce the concept of minimum requirements Default to the use of the data Reorganized QC section to “before” and “during” analysis, for example: Media Checks: Before Blanks: During

2016 Radiochemistry Standard Volume 1, Module 6

Background The laboratory community is familiar with “stable” chemistry Environmental testing protocols for inorganic and organic evolved separately Some of these protocols and concepts are less applicable to radiochemistry Volume 1, Module 6

Regulatory Background Only one formalized program (EPA Laboratory Certification for Water) Narrow and specific set of parameters for water Methods based on 1950 s -1980 s EPA lab procedures Technology has changed Instruments and even reagents not always available Little or no performance/validation data Peculiar biases specific to SDWA and CWA compliance Quality requirements sparse (to put it politely…)

What are Some Key Differences? Isotopic measurements of radionuclides Lab-developed, performance-based methods Measurements relative to background Reported Chemical separations with yield tracers “As measured” - positive, negative or zero Not censored against IDL, MDL, RL! The measurement uncertainty is calculated and reported together with each result

“MARLAP” Cross-agency document developed and approved by eight federal agencies: ª EPA, DOD, DOE, DHS, NRC, FDA, USGS, NIST u u Part I for project planners / managers of radioanalytical projects Parts II and III address technical topics Very worthwhile !!!

Radiochemistry Expert Committee Formed in 2012 Consists of 10 radiochemists Extensive experience in operation and oversight of state, federal, and commercial laboratories Reviewed and updated TNI Standard Module 6 The Voting Draft Standard was successfully balloted in April 2015

Radiochemistry Standard 1. 1 Introduction 1. 2 Scope 1. 3 Terms and Definitions 1. 3. 1 Additional Terms and Definitions 1. 3. 2 Exclusions and Exceptions 1. 4 Method Selection 1. 5 Method Validation 1. 5. 1 1. 5. 2 1. 5. 3 1. 5. 4 1. 5. 5 Validation of Methods Detection Capability Evaluation of Precision and Bias Measurement Uncertainty Evaluation of Selectivity Volume 1, Module 6 1. 6 Demonstration of Capability 1. 6. 1 General 1. 6. 2 Initial DOC 1. 6. 3 Ongoing DOC 1. 7 Technical Requirements 1. 7. 1 Instrument Set-up, Calibration, Performance Checks, and Background Measurements 1. 7. 2 Quality Control for Radiochemistry 1. 7. 3 Data Evaluation and Reporting 1. 7. 4 Sample Handling

Major Changes Definitions for key terms were added to Section 1. 3. Requirements for method validation in Section 1. 5 were refined to better address laboratorydeveloped/modified methods and to evaluate uncertainty and method performance at background (zero) activity. Section 1. 6 requirements for Demonstrations of Capability include analysis of blanks, once again to address method performance at background activity. Technical requirements in Section 1. 7 were reorganized to logically parallel set-up, calibration verifications, and quality control of instrumentation. V 1 M 6

Major Changes (Cont. ) Section 1. 7. 1 provides requirements for mathematical calibration methods, and for several approaches to background determination, both of which are in common use but neither of which are currently permitted. The most substantial change to method quality controls in Section 1. 7. 2, the Radiation Measurements Batch, was introduced to eliminate substantial confusion, and inconsistent implementation of batch quality controls for non-destructive analyses such as gamma spectrometry. Section 1. 7. 3 contains requirements for evaluating chemical yield which were not included in previous revisions. It also addresses reporting requirements for uncertainty. V 1 M 6

The 2016 TNI Standard Changes to PT, Quality Systems, Chemistry, Microbiology and Radiochemistry Also changes to Volumes 2, 3, and 4 Expected to be fully adopted by CSDP by October 2016. Will need review by LASEC for suitability Will need adoption by NELAP for implementation NELAP implementation will be for a specific date, likely 2018

Implementation of 2016 TNI Standard 2 -3 year process Extensive training will be provided to labs and lab assessors New checklists and guidance will be developed Quality Manual template will likely be revised

Contact TNI Jerry Parr, Executive Director www. nelac-institute. org jerry. parr@nelac-institute. org 817 -598 -1624