a systematic approach to the analysis of general...
TRANSCRIPT
![Page 1: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/1.jpg)
A Systematic Approach to the
Analysis of General Unknowns
Vincent J. Desiderio
New Jersey State Police
Office of Forensic Sciences
![Page 2: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/2.jpg)
The Great State of New Jersey
![Page 3: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/3.jpg)
The Great State of New Jersey
![Page 4: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/4.jpg)
The Great State of New Jersey
![Page 5: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/5.jpg)
The Great State of New Jersey
![Page 6: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/6.jpg)
The Great State of New Jersey
![Page 7: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/7.jpg)
The Great State of New Jersey
![Page 8: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/8.jpg)
The Great State of New Jersey
![Page 9: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/9.jpg)
The Great State of New Jersey
![Page 10: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/10.jpg)
The Great State of New Jersey
![Page 11: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/11.jpg)
General
Unknowns
• Reasons for Submission:
– Identification of contents
– Determination if specific compound(s) is/are
present
– Determination if a questioned substance is
comparable to a known
– Routine case takes a turn
![Page 12: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/12.jpg)
![Page 13: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/13.jpg)
![Page 14: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/14.jpg)
General
Unknowns
• Role of Analyses:
– Provide links between:
• Victim & Suspect
• Victim & Scene
• Suspect & Scene
– Provide proof of a criminal act.
– Provide investigative leads.
– Support or refute a story.
– Provide information for reconstructions.
![Page 15: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/15.jpg)
Common
Submissions
• Unknown powders
• Unknown liquids
• Unknown mixtures
• Items with unknown residues
• Solids thought to contain adulterants
• Liquids thought to contain adulterants
![Page 16: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/16.jpg)
Common
Analytes
• Inorganic salts
• Building materials
• Acids
• Bases
• Greases
• Oils
• Cleaning products
• Bleach
• Volatile organics
• Solvents
• Pesticides
• Random schmutz
![Page 17: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/17.jpg)
General
Considerations
• Safety first
• Is there any background information?
• Analysis requires a well thought out approach
– No single way to approach any given case
– Experience and common sense are important
• Often utilize every available resource
• Can be literally anything, but often something
common
![Page 18: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/18.jpg)
Case Example
• Background:
– Suspect is an illegal alien looking to purchase a
large quantity of “Ammonium Nitrate”
– White powder found in vehicle
– Visual/Stereomicroscopic exam indicated
powder was finely ground and uniform
– Proceeded to use EDXRF for elemental
analysis
![Page 19: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/19.jpg)
Case Example
![Page 20: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/20.jpg)
Case Example
• Elemental profile of sample indicated the
presence of lime
• This was then confirmed using X-Ray
Diffraction
![Page 21: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/21.jpg)
Systematic
Approach
• The Analytical Funnel:
– Start with general approach and compile information
– Narrow down possibilities with ultimate goal of
identification
General
Observations
Microscopy
Screening
Techniques
Molecular
Identification
![Page 22: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/22.jpg)
Systematic
Approach
• Analytes can be broken down into solids,
liquids, and gases
• Each of which may contain single
components, homogenous mixtures (e.g.
liquid solutions), or heterogeneous mixtures
(e.g. mixed crystalline compounds)
![Page 23: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/23.jpg)
Systematic
Approach
• General Observations:
– Packaging (commercial container, condition of
container, listed ingredients, markings, etc.)
– State of sample (solid, liquid, gas, mixture)
– General amount of sample present
– Obvious odor
![Page 24: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/24.jpg)
Solids
• Visual/General Examination
– Color
– Consistency (e.g. metallic, powder, resin, polymeric,
etc.)
• Stereomicroscopic Examination
– Crystalline vs. Amorphous
– Organic vs. Inorganic
– Homogenous vs. Heterogeneous
• Manual separation of particles
![Page 25: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/25.jpg)
Solids
• Light Microscopy/Polarized Light Microscopy
– Color with transmitted light
– Homogenous vs. Heterogeneous
– Isotropic vs. Anisotropic
– Presence of pigments/fillers
– General refractive index
– Particle identification
![Page 26: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/26.jpg)
Solids
• Ignition test (low explosives, improvised
explosive mixtures)
• Chemical Tests
– Solubility
– Spot Tests/Color Tests
– Crystal Tests
![Page 27: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/27.jpg)
Solids
• Instrumentation:
– Elemental Analysis: EDXRF, SEM-EDS
– GC, GC/MS (Organics)
– Pyrolysis GC, GC/MS
– FTIR
– XRD
![Page 28: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/28.jpg)
Solids
• General Approach:
1) Visual/General Examination
2) Stereomicroscopic Examination
3) PLM
4) Elemental Analysis (organic vs.inorganic)
5) Compound Identification
a) FTIR
b) XRD
c) Mass Spectrometry (GC/MS, Py-GC/MS)
6) Additional tests
a) Chemical Tests
b) Ignition Tests
![Page 29: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/29.jpg)
Liquids
• Visual/General Examination
– Color
– Single vs. Multi Phase (organic/aqueous mix)
– General viscosity
– Presence of any precipitate or sediment
• pH
• Conductivity (Ionic Solution)
• Ignition Test (Ignitable Liquid)
![Page 30: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/30.jpg)
Liquids
• Solid-Liquid Solution
• Liquid-Liquid Solution
• Extractions
– Liquid-Liquid
– Acid/Base
– Solid Phase Extraction
– Precipitation
– Evaporation/Distillation
– Heated and Passive Headspace (volatile organics)
![Page 31: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/31.jpg)
Liquids
• Chemical tests
– Precipitate Reactions
– Spot Tests
– Color Tests
– Crystal tests
• Instrumental Analysis
– Elemental Analysis
• EDXRF (in absence of vacuum)
• SEM-EDS (precipitates only)
![Page 32: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/32.jpg)
Liquids
• Instrumental Analysis (cont.)
– GC, GC/MS (organic solutions, extracts)
– FTIR
• Liquid samples (liquid cell, ATR)
• Precipitates
– XRD
• Precipitates
![Page 33: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/33.jpg)
Liquids
• General Approach:
1)Visual/General Examination
2) pH
3)Conductivity
4)Ignition Test
5)Extraction/Solvent Dilution/Evaporation/Precipitation
6)Sample Screening/Identification of Components
a)FTIR
b)Mass Spectrometry (GC/MS, Py-GC/MS)
c)Elemental Analysis
7)Chemical Tests
![Page 34: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/34.jpg)
Elemental Analysis of Liquid (EDXRF w/o Vacuum)
![Page 35: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/35.jpg)
Swab Blank (EDXRF w/o Vacuum)
![Page 36: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/36.jpg)
Gases
• Rarely Encountered
• Safety Concerns
• Analysis
– GC, GC/MS
– FTIR via Gas Cell
![Page 37: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/37.jpg)
Elemental
Analysis
• Organic vs. Inorganic
• Elemental composition
• Preliminary information for screening
purposes
• SEM-EDS vs. EDXRF
![Page 38: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/38.jpg)
Special
Considerations
• Consider any chemistry
• Controls and
Comparisons
• Hydration States
– Desiccation, Baking Out
• Hydroscopic Salts
– Dry and coat with mineral/silicone oil
• Small amounts of
analyte: scale down
tests
• Rely on others
– Ask questions
– Make calls
• Sometimes it just
doesn’t work out!
![Page 39: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/39.jpg)
Case Examples
![Page 40: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/40.jpg)
Beefcake 4000
![Page 41: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/41.jpg)
Beefcake 4000
![Page 42: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/42.jpg)
A Cup of Joe
![Page 43: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/43.jpg)
A Cup of Joe
• Suspect is accused of adding cupric sulfate
to instant coffee
• Victim prepares a cup of joe that doesn’t
taste so good
![Page 44: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/44.jpg)
Cup of Joe
![Page 45: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/45.jpg)
Cup of Joe
![Page 46: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/46.jpg)
Cup of Joe
![Page 47: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/47.jpg)
The Anarchist
![Page 48: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/48.jpg)
The Anarchist
• Background:
• Suspect had an anarchist cookbook sampler
– Plastic water bottle with white slurry and what
appeared to be balls of aluminum foil
– Gray powder (“Explosive Powder”)
– Incendiary device (analyzed as fire debris)
![Page 49: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/49.jpg)
EDXRF vs. SEM-EDS
![Page 50: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/50.jpg)
EDXRF vs. SEM-EDS
![Page 51: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/51.jpg)
EDXRF vs. SEM-EDS
![Page 52: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/52.jpg)
The Anarchist
• Gray powder (“Explosive Powder”)
– Visual/Stereomicroscopic examination
disclosed the presence of gray and beige
granules as well as clear crystals
– Ignition test negative
– Proceeded to analyze using EDXRF and SEM-
EDS
![Page 53: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/53.jpg)
The Anarchist
• Gray powder:
![Page 54: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/54.jpg)
The Anarchist
• Gray powder EDXRF:
![Page 55: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/55.jpg)
The Anarchist
• Conclusions:
– Gray Powder
• Clear crystals had rhombohedral shape
characteristic of sucrose. Confirmed sucrose
using FTIR.
• Mixture of arsenic and sugar indicated that
this sample was rat poison.
![Page 56: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/56.jpg)
Mmmm Lunch!
![Page 57: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/57.jpg)
Mmmm Lunch
• Background:
–Husband Suspects Wife of Poisoning
His Prepared Lunch Consisting Of:
• Buffalo Style Chicken Wings
• Coffee
![Page 58: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/58.jpg)
Mmmm Lunch
![Page 59: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/59.jpg)
Mmmm Lunch
![Page 60: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/60.jpg)
Mmmm Lunch
Coffee Chromatogram
Coffee Aromatic Profile
![Page 61: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/61.jpg)
Mmmm Lunch
Coffee (Insecticide)
Coffee (Insecticide) Mass Spectrum
![Page 62: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/62.jpg)
Mmmm Lunch
![Page 63: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/63.jpg)
Glade
![Page 64: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/64.jpg)
Glade
• Background:
– Partially decomposed female victim found in basement
of boarding house covered with white powder
– Victim’s husband was the the main suspect
– A sample of the white powder was collected at scene
and submitted for identification
– Prosecution theory: The husband killed his wife and hid
her in the basement. Covered her with white powder to
hide odor.
![Page 65: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/65.jpg)
Glade
• The white powder was received in the lab and
opened.
• A sweet, distinct odor was immediately noticed.
• Analysis proceeded as follows: Visual/
stereomicroscopic examination, elemental
analysis, FTIR, XRD.
• Results: Primarily inorganic, containing sodium
sulfate.
![Page 66: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/66.jpg)
Glade
• Background research indicated a possible carpet deodorizer
• Proceeded to reference collection
• Shop-Rite across the street
• Looked a bit crazy for a while in the cleaning supplies aisle looking at ingredients and sniffing various carpet deodorizer bottles
• Found one that had a comparable odor, purchased and brought it back to the lab for analysis
![Page 67: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/67.jpg)
Glade
• Performed same analyses and observed comparable results
• Extracted both the unknown and reference sample
for GC-MS analysis.
• Observed to contain similar components (Jasmine Oil)
• Report: The white powder contains sodium sulfate
and a fragrance component. Substances which contain such mixtures include but are not limited to some carpet deodorizers.
![Page 68: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/68.jpg)
Elemental
Analysis
![Page 69: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/69.jpg)
FTIR
![Page 70: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/70.jpg)
XRD
Unknown White Powder
![Page 71: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/71.jpg)
GC-MS
Glade Carpet Deodorizer
Unknown White Powder
![Page 72: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/72.jpg)
Glade
• In validation of the conclusion, after the
report was issued, it was disclosed that the
suspect admitted to his cellmate that he had
sprinkled carpet deodorizer on the victim to
hide the odor.
![Page 73: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/73.jpg)
Resources
![Page 74: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/74.jpg)
Resources
![Page 75: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/75.jpg)
Resources
![Page 76: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/76.jpg)
Resources
![Page 77: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/77.jpg)
Resources
![Page 78: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/78.jpg)
Resources
![Page 79: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/79.jpg)
Resources
![Page 80: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/80.jpg)
Resources
![Page 81: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/81.jpg)
Resources
![Page 82: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/82.jpg)
Resources
![Page 83: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/83.jpg)
References
• http://webbook.nist.gov/chemistry/
• http://householdproducts.nlm.nih.gov/
• http://riodb01.ibase.aist.go.jp/sdbs/cgi-bin/
cre_index.cgi?lang=eng
![Page 84: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/84.jpg)
Acknowledgements
• Dr. Howard Baum
• Ajit Tungare
• Jacki Mancilla
• George W. Chin
• Melissa Balogh, Stew Hung, and Jayne DeMichelle
• Cassandra Burke and the Symposium Steering
Committee
• Jocelyn Williams
• Katie Ballance and The Pink Gorilla Dude
![Page 85: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/85.jpg)
Questions?
![Page 86: A Systematic Approach to the Analysis of General …projects.nfstc.org/trace/2009/presentations/6-desidero-systematic.pdfA Systematic Approach to the Analysis of General Unknowns](https://reader031.vdocuments.mx/reader031/viewer/2022022005/5ab7ae3b7f8b9ad3038be86d/html5/thumbnails/86.jpg)
Questions?