Drug Enforcement Administration Office of Forensic Sciences Analysis of Drugs Manual September 2019 Date Posted: 10/23/2019 Analysis of Drugs Manual Revision: 4 Issue Date: September 5, 2019 Effective Date: September 9, 2019 Approved By: Nelson A. Santos Table of Contents CHAPTER 1 – QUALITY ASSURANCE ......................................................................... 3 CHAPTER 2 – EVIDENCE ANALYSIS ......................................................................... 93 CHAPTER 3 – FIELD ASSISTANCE .......................................................................... 165 CHAPTER 4 – FINGERPRINT AND SPECIAL PROGRAMS ..................................... 179 Appendix 1A – Definitions ........................................................................................... 202 Appendix 1B – Acronyms and Abbreviations .............................................................. 211 Appendix 1C – Instrument Maintenance Schedule ..................................................... 218 Appendix 1D – Color Test Reagent Preparation and Procedures ............................... 224 Appendix 1E – Crystal and Precipitate Test Reagent Preparation and Procedures .... 241 Appendix 1F – Thin Layer Chromatography................................................................ 250 Appendix 1G – Qualitative Method Modifications ........................................................ 254 Appendix 1H – Analytical Supplies and Services ........................................................ 256 Appendix 2A – Random Sampling Procedures ........................................................... 257 Appendix 2B – Reporting Statements ......................................................................... 259 Appendix 2C – Composite Formation Procedures ...................................................... 262 Appendix 2D – Methamphetamine Isomer Reporting .................................................. 265 Appendix 2E – Procedures for the Germination and Analysis of Marijuana Seeds ..... 266 Appendix 2F – Uncertainty of Measurement Estimates .............................................. 268 Appendix 2G – Instructions for Completing LIMS Tests .............................................. 276 REDACTED ................................................................................................................ 298 TABLE 1 ...................................................................................................................... 299 TABLE 2 ...................................................................................................................... 300 SOP-CH-001 ............................................................................................................... 302 End of Document ........................................................................................................ 314 2 Date Posted: 10/23/2019 Analysis of Drugs Manual Chapter 1 – Quality Assurance Revision: 4 Issue Date: September 5, 2019 Effective Date: September 9, 2019 Approved By: Nelson A. Santos CHAPTER 1 – QUALITY ASSURANCE 1.0 Quality Assurance ............................................................................................... 9 1.1 Scope .......................................................................................................................... 9 1.2 Definitions and Abbreviations ....................................................................................... 9 2.0 Proficiency Testing Program ............................................................................ 10 2.1 Preparing Proficiency Samples ...................................................................................10 2.1.1 Preparing Proficiency Samples of Known Composition ........................................10 2.1.2 Preparing Proficiency 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 ...........................................................................................19 2.5 Laboratory Blind Proficiency Test Samples .................................................................20 3.0 Validating Qualitative Instrumental Methods .................................................. 21 3.1 Validating Qualitative Separation Methods ..................................................................23 3.1.1 Selectivity ............................................................................................................23 3.1.2 Repeatability (Short-term Precision) ....................................................................26 3.1.3 Reproducibility (Long-term Precision) ..................................................................27 3.2 Validating Qualitative Confirmatory Methods...............................................................29 3.2.1 Accuracy ..............................................................................................................29 3 Date Posted: 10/23/2019 Analysis of Drugs Manual Chapter 1 – Quality Assurance Revision: 4 Issue Date: September 5, 2019 Effective Date: September 9, 2019 Approved By: Nelson A. Santos 3.3 Supplementing Original Validation Documentation......................................................33 3.4 Validating the Cannabis Analysis Separatory Method .................................................34 3.4.1 SFL1 Validation Procedures ................................................................................34 3.4.2 Field Laboratory Validation Procedures ...............................................................34 3.4.3 Ruggedness Testing .............................................................................................35 3.5 Ad hoc Validation of Qualitative Instrumental Methods ...............................................35 4.0 Developing and Validating Quantitative Separation Methods ....................... 37 4.1 Proposing a New Quantitative Separation Method ......................................................37 4.2 Validating Quantitative Separation Methods................................................................38 4.3 Levels of Validation for Quantitative Separation Methods ...........................................39 4.3.1 Level 1 .................................................................................................................39 4.3.2 Level 2 .................................................................................................................39 4.3.3 Level 3 .................................................................................................................39 4.3.4 Level 4 .................................................................................................................39 4.3.5 Validation Scheme Summary ...............................................................................40 4.4 Selectivity ...................................................................................................................40 4.4.1 Evaluation Procedures .........................................................................................40 4.4.2 Acceptance Criteria..............................................................................................41 4.4.3 Reporting Requirements ......................................................................................41 4.5 Linearity ......................................................................................................................41 4.5.1 Evaluation Procedures .........................................................................................41 4.5.2 Data Evaluation ...................................................................................................42 4.5.3 Preparing a Sensitivity Plot ..................................................................................42 4.5.4 Examples of Regression and Sensitivity Plots ......................................................43 4.5.5 Acceptance Criteria..............................................................................................43 4.5.6 Reporting Requirements ......................................................................................43 4.6 Repeatability