Drug Enforcement Administration Office of Forensic Sciences Analysis of Drugs Manual April 2018 Date Posted: April 27, 2018 Analysis of Drugs Manual Revision: 3 Issue Date: April 24, 2018 Effective Date: April 24, 2018 Approved By: Nelson A. Santos Table of Contents CHAPTER 1 – QUALITY ASSURANCE .......................................................................... 3 CHAPTER 2 – EVIDENCE ANALYSIS ......................................................................... 87 CHAPTER 3 – FIELD ASSISTANCE .......................................................................... 158 CHAPTER 4 – FINGERPRINT REDACTED ............................................................... 170 Appendix 1A – Definitions ........................................................................................... 193 Appendix 1B – Instrument Maintenance Schedule ...................................................... 202 Appendix 1C – Color Test Reagent Preparation and Procedures ............................... 208 Appendix 1D – Crystal and Precipitate Test Reagent Preparation and Procedures .... 224 Appendix 1E – Thin Layer Chromatography ............................................................... 232 Appendix 1F – Qualitative Method Modifications ........................................................ 236 Appendix 1G – Critical Consumables, Services, and Supplies ................................... 238 Appendix 2A – Random Sampling Procedures ........................................................... 239 Appendix 2B – Reporting Statements for Net Weight Determination, Identification(s), and Purity Result(s) ..................................................................................................... 241 Appendix 2C – Composite Formation Procedures ...................................................... 244 Appendix 2D – Methamphetamine Isomer Reporting .................................................. 247 Appendix 2E – Procedures for the Germination and Analysis of Marijuana Seeds ..... 248 Appendix 2F – Uncertainty of Measurement Estimates............................................... 250 Appendix 2G – Instructions for Completing LIMS Tests .............................................. 258 REDACTED ................................................................................................................ 280 TABLE 1 ...................................................................................................................... 281 TABLE 2 ...................................................................................................................... 282 End of Document ........................................................................................................ 284 2 Date Posted: April 27, 2018 Analysis of Drugs Manual Chapter 1 – Quality Assurance Revision: 3 Issue Date: April 24, 2018 Effective Date: April 24, 2018 Approved By: Nelson A. Santos CHAPTER 1 – QUALITY ASSURANCE 1.0 Quality Assurance ............................................................................................... 9 1.1 Scope .......................................................................................................................... 9 1.2 Definitions .................................................................................................................... 9 2.0 Proficiency Testing Program ............................................................................ 10 2.1 Preparing PTP and IPTP Samples ..............................................................................10 2.1.1 Preparing PTP and IPTP Samples of Known Composition...................................10 2.1.2 Preparing PTP and IPTP Samples from Evidence ...............................................11 2.2 Inter-Laboratory Proficiency Test Samples .................................................................12 2.2.1 Preparing PTP Samples ......................................................................................13 2.2.2 Packaging and Distributing of PTP Samples ........................................................13 2.2.3 Analyzing PTP Samples and Reporting Results ...................................................14 2.2.4 Documenting the PTP ..........................................................................................15 2.3 Internal Proficiency Test Samples ...............................................................................17 2.3.1 Preparing IPTP Samples .....................................................................................17 2.3.2 Packaging and Distributing IPTP Samples ...........................................................18 2.3.3 Documenting IPTP Results ..................................................................................18 2.3.4 Evaluating IPTP Results ......................................................................................19 2.3.5 Reporting IPTP Results .......................................................................................19 2.4 External Proficiency Test Samples ..............................................................................19 2.4.1 Completing an EPTP ...........................................................................................20 2.5 Laboratory Blind Proficiency Test Samples .................................................................20 2.6 Clandestine Laboratory Type Proficiency Test Samples .............................................21 2.6.1 Preparing Clandestine Laboratory-Type Proficiency Samples ..............................21 3.0 Validating Qualitative Instrumental Methods .................................................. 22 3.1 Validating Qualitative Separation Methods ..................................................................24 3.1.1 Selectivity ............................................................................................................24 3.1.2 Repeatability (Short-term Precision) ....................................................................26 3.1.3 Reproducibility (Long-term Precision) ..................................................................28 3 Date Posted: April 27, 2018 Analysis of Drugs Manual Chapter 1 – Quality Assurance Revision: 3 Issue Date: April 24, 2018 Effective Date: April 24, 2018 Approved By: Nelson A. Santos 3.2 Validating Qualitative Confirmatory Methods...............................................................29 3.2.1 Accuracy ..............................................................................................................29 3.3 Supplementing Original Validation Documentation......................................................33 4.0 Developing and Validating Quantitative Separation Methods ....................... 35 4.1 Proposing a New Quantitative Separation Method ......................................................35 4.2 Validating Quantitative Separation Methods................................................................36 4.3 Levels of Validation for Quantitative Separation Methods ...........................................37 4.3.1 Level 1 .................................................................................................................37 4.3.2 Level 2 .................................................................................................................37 4.3.3 Level 3 .................................................................................................................37 4.3.4 Level 4 .................................................................................................................37 4.3.5 Validation Scheme Summary ...............................................................................38 4.4 Selectivity ...................................................................................................................38 4.4.1 Evaluation Procedures .........................................................................................38 4.4.2 Acceptance Criteria..............................................................................................39 4.4.3 Reporting Requirements ......................................................................................39 4.5 Linearity ......................................................................................................................39 4.5.1 Evaluation Procedures .........................................................................................39 4.5.2 Data Evaluation ...................................................................................................40 4.5.3 Preparing a Sensitivity Plot ..................................................................................40 4.5.4 Examples of Regression and Sensitivity Plots ......................................................41 4.5.5 Acceptance Criteria..............................................................................................41 4.5.6 Reporting Requirements ......................................................................................41 4.6 Repeatability ...............................................................................................................42 4.6.1 Evaluation Procedures .........................................................................................42 4.6.2 Acceptance Criteria..............................................................................................42 4.6.3 Reporting Requirements ......................................................................................43 4.7 Accuracy .....................................................................................................................43