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1. Introduction
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Forensic Laboratory Basic Intern
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Forensic Laboratory Basic Intern
Contents
1. Introduction
1.1 Intro to the Online Version
1.2 Schedule
2. Introduction to Infrared Spectroscopy
2.1 General Theory of Infrared Absorption
2.1.1 Atomic Oscillators
2.1.2 Quantum Oscillators
2.1.3 Polyatomic Oscillators
2.1.4 Allowed transitions in IR spectroscopy
2.1.5 Spectroscopy
2.2 Group Regions
2.3 Common Sampling Modes
2.4 Sampling Techniques Used in This Lab
2.4.1 Diffuse Reflectance
2.4.2 Horizontal Attenuated Total Reflectance
2.4.3 Units for Reflectance Spectra
2.5 OMNIC Software Overview
2.6 Links to IR Web Sites
3. Extraction Techniques
3.1 Introduction to Extractions
3.2 Liquid-Solid Extraction
3.3 Liquid-Liquid Extraction
3.3.1 Partitioning
3.3.2 Acid-Base Extractions
3.3.3 Applying acid-base extraction
3.3.4 Further comments on acid-base extraction
4. Basic GC Theory
4.1 What use is a GC?
4.2 How a GC Separates
4.2.1 Basic Chromatography Theory
4.2.2 Summarizing Solute Retention
4.2.3 Retention Index and Relative Interactions with Stationary Phase
4.3 Sample Introduction Into the Gas Chromatograph
4.3.1 Basic Inlet Techniques
4.3.2 Other Inlet Techniques
4.3.3 Manual Injection vs. Automatic Injection
5. General Mass Spectrometry Theory
5.1 Overview of Mass Spectrometry
5.2 Ionization
5.2.1 The Ionization Process
5.2.2 Energetics of Electron Impact Ionization
5.2.3 The Energetics of Fragmentation
5.3 Mass Analysis
5.3.1 Mass Analysis by Ion Time-Of-Flight
5.3.2 Mass Analysis by Magnetic Fields
5.3.3 Mass Analysis by Quadrupole Fields
5.3.4 Mass Analysis by Ion Cyclotron Resonance
5.3.5 Tandem and Hybrid Techniques
5.4 Ion Detection
5.4.1 Electron Multipliers
5.4.2 Other Ion Detection Techniques
5.5 Vacuum Systems
5.5.1 Rough Vacuum
5.5.2 High vacuum
5.5.3 Ultra High Vacuum
5.6 General Appearance of a mass spectrum
6. Mass Spectra Interpretation I
6.1 Molecular Mass
6.1.1 Assignment of the Molecular Ion
6.1.2 Molecular Mass Determination for Total Unknowns
6.1.3 The Nitrogen Rule
6.1.4 Exercise-MI Assignment
6.2 Origin of Molecular Ion Decomposition Reactions
6.2.1 Ionization
6.2.2 Charge Site Influences the Reaction Site
6.2.3 Competing Reactions
6.2.4 Overall Chemistry
6.3 Simple Cleavage Reactions
6.3.1 A Simple Reacting Molecule
6.3.2 Sequential Simple Cleavages
6.3.3 Logical Neutral Radical Losses
6.3.4 Stability Order of Cations and Radicals
6.3.5 Exercises
7. Overview of the GC/MS Data System
7.1 Basic System Architecture
7.2 Methods
7.3 Some How-To's of Manipulating MS data
7.3.1 Total Ion Chromatogram
7.3.2 Extracted Ion Chromatogram
7.3.3 Mass Spectrum of a Single Scan
7.3.4 Average Mass Spectra
7.3.5 Zooming the Display Chromatographic and Mass Spectral Data
7.3.6 Subtracting Background Spectra
7.3.7 Library Searching
7.3.8 Extracting Spectra from the Library
8. Mass Spectra Interpretation II
8.1 Isotope Peaks
8.1.1 What are Isotope Peaks?
8.1.2 Definition of the Atomic Mass Scale and Average Masses
8.1.3 What Mass Does the Mass Spectrometer Measure?
8.1.4 Isotope Peaks as a Criterion For Signal Integrity
8.2 Rearrangement Reactions
8.2.1 A Convention for Moving Electrons in Reaction Mechanism Diagrams
8.2.2 Product Stabilization by Rearrangement
8.2.3 Retro Reactions
8.2.4 McLafferty Rearrangement
8.3 Complete Mechanisms for Observed Product Ion Signals
8.4 Group/Class Series
9. Sample Preparation for GC/MS
9.1 Target Concentrations for General Purpose Analysis
9.2 Dynamic Range in Sensitivity
9.3 Acid-Base Forms of Organic Analytes
10. Identity Confirmation by Mass Spectrometry
10.1 Required Information to Confirm and Identity
10.2 Ancillary Information to Aid Identity Confirmation
11. Forensic Analysis Training
11.1 Evidence Handling - Chain of Custody
11.2 Documentation
11.2.1 Instrument Logs
11.2.2 The Analysis Worksheet
11.2.3 Analysis Report
11.2.4 Keeping Notes
11.3 Testing Evidence
11.3.1 Presumptive Testing
11.3.2 Confirmatory Tests for Identification
12. Additional Reading
John S. Riley,
DSB Scientific Consulting
