forensic applications of sem/edx, p-xrf and xrd at the national...
TRANSCRIPT
The Abdus Salam1tIjII International Centre for Theoretical PhysicsPl
IAEA
SMRII843-5
X-Ray Emission Techniques for Forensic Applications
28 May - 1 June, 2007
ForensicApplicalionsof SEMJEDX ji-XRF andXRDattheNafionatlns&uteofForensic Science
Bart NysNational Insitute for Criminalistics and Criminology,
Brussels - Belgium
Strada Costiera II. 34014 Trieste, Italy -Tel *39 040 2240 11 I Fax *39 040 224 163 - sci irsfo@ictp it, wwwictp it
-tA
Nationaal Instituut voorCriminalistiek en CriminologieJustitie
Forensic Applicationsof SEM/EDX, p-XRF and XRD at the
National Institute of Forensic Science
. .Forensic Researcher
Chemical Ballistics Lab
Bart Nys May 2007
aqoLOOJcJAIS/MJI
AqdejboeE)
aqoLOOJcJAISJcNJI
ooo'ooo'o:uoipJndofcSJfMM+:zis
AqdejboeE)
History
" First Laws Passed in 1971
" Founded in 1992
" Personnel Evolution: 7 (1992) - 70 (1995) - ±130 (since 2000)
" Expansion of Laboratories: 4 (1992) to 9 (since 1995)
" Number of Court Cases: ± 40,000 since 1992
Bart Nys May 2007
Organisation Context
Bart Nys May 2007
Our Mission
" Examination of Evidence collected at a Crime Scene
" Research and Development of Forensic Techniques
" Compilation of Databases of Forensic Data
" Studies in Criminology and Police Policy Making
*Training and Education of Police Lab Operatives
" Central Lab facillity of the Department of Justice
Bart Nys May 2007
Forensic Domains
"Drugs & Toxicology
" DNA typing - Database
I" Microtraces - Entomology
" Fibres, Arson & Materials
Analysis7
" Chemical Ballistics (i" Ballistics & Toolmarks
Bart Nys May 2007
Organisation StructureI Head of Institute U
DivisionTechnical Assistance
Division
Quality Assurance
Division
Management
artment
Criminology
IDivisionICT
Division
Accounting
National DNA Database
I DepartmentForensics
BallisticsI Division
National Ballistics
I
LabChemical Ballistics
Mechanical Ballistics II Lab
I Division
Analytical Chemistry
Arson Material Analysis
Lab
Fibres
I Division
Biology
I
Lab
Bi otraces DNA TypingI Lab
I Division
Drugs & Toxicology
Drugs AnalysisI Lab
ToxicologyI Lab
Bart Nys May 2007
Quality Assurance
" ISO 17025
" DNA lab Accreditation in 2004
" Other Labs to follow (TOX 2006, ...)
" Development of Procedures, Documents
" Databases for Document and Case Management
Bart Nys May 2007
Routine Activities" Casework in GSR analysis:
" SEM Analysis of GSR using our own Sampling Kit"Development of the GSR Database (European project)
" Sheet Printing Method on Clothing and other Objects
" Development of new Techniques:" SEM Analysis of Light Bulb Filaments" Entomology" Document Analysis" Glass Analysis"
" Services to other Labs" Material Analysis" Fibres Analysis" Ballistics (p-Toolmarks)
Bart Nys May 2007
Lab Infrastructure
Benchtop
Zone 2 RI .
Zone 1
Benchtop
Zone 2010F- R2
R3 Zone i
r
Zone 0
SEM2
AreaSEMiArea
RI
Zone 2
Labs
aBenChI0p
Bart Nys May 2007
a H
Gunshot Residue Application
((GSR: Gun Shot Residue))((FOR: Firing Discharge Residue PDR: Primer Discharge Residue))
Bart Nys May 2007
Gunshot Residues are microscopic and macroscopicParticles formed during the firing process, originating
from both Powder and Primer Components
aqoLOOZ'J'\I
JOPMOdUflD
JOW!Jd
!
ALL*.o6pup
WNW-
s/cMJ1S3
ioiin
UO1IflIJSUOO7
UOqB3!ddOflp!SOHloqsunE)
Gunshot Residue Application
Deposition
Sides
Shooter
Hands
Clothing
Face - Hair (rifle)
Shooting Environment
uzzle
Target
Clothing
Objects in Vicinity
Bart Nys May 2007
aqoLOOJcJAIS/MJI
JO1OWOJ3!W019-0:Oz!sO6JOAV
uoileo!lddVanp!sa~jloqsunE)
Gunshot Residue Applicationi Classification:
01 TargetShooter
MicroscopicGunshot Residi
MacroscopicGunshot Residue
Chemographic Tests
But also
GSR KitMicroscopic
Gunshot Residue
Electron Microscopy
Bart Nys May 2007 be
Gunshot Residue Applicationi Classification
I Metallic GSR
Primer, Bullet, Cartridge
I Organic GSR
Gun Powder
- Lead, barium, antimony
- Titanium, zinc (Sintox)
- Strontium, zirconium
Explosives and Additives
Research
Project+ Copper, Zinc, Nickel, Calcium,
1Routine CaseRoutine CaseWorkWork
Bart Nys May 2007
aqoLOOJcJAI
S/MJI
peidwesosieeiese6p!Jpeoeoueiejeipue6uqoospedsns'eqssodii
6uiidwespue6u!J!jueeivqeqpedsnsjOse!!A!pepueewieqeououepodwi
BuildweSPUSH_#
uoileo!lddVanp!sa~jloqsunE)
Gunshot Residue ApplicationAnalysis
- Automated scanning of Stub Area
Detection of Particles using BSE
EDX Spectrum Acquisition
- Automatic Classification of Particles
- After Analysis: manual review of found
Particles
- Total Analyis Time required per Kit:
I to 3 days
Bart Nys May 2007
aqoLOOJcJAIS/MJI
A6ooqdo013!pBdso6wiElSe
s;nsej
uoileo!lddVanp!sa~jloqsunE)
Gunshot Residue ApplicationResults
Classification of Particles:
- Unique - Characteristic: Pb/Ba/Sb in one Particle
((Classic)) Approach - Probable: Pb/Ba, Pb/Sb, Ba/Sb in one Particle
- Indicative: Pb containing Particles
- Comparisons based on recovered Cartridges,Now and in the Future Ammunitions, Firearms
- Searches using Databases of Primer Composition
Bart Nys May 2007
Gunshot Residue Database
" "What type of ammunition is this?"" "Is the ammunition used in this case the same as in
this other case?"" "Was this type of particle ever seen in GSR samples
before?"
* Catalogue of ammunition
evelopment of new processing methods
Correlation between analysis methods
Bart Nys May 2007
Survey - Participants
" Austria" Deutschland (BKA)" Deutschland (LKA Sachsen-Anhalt)" Deutschland (LKA Berlin)" Espana" Espana" Finland" France" Greece" Israel" Italy" Lithuania
NetherlandsN-IrelandPoland
PortugalSchweiz (Zurich)Schweiz (St. Gallen)SlovakiaSuisse (ECRA)SwedenUK (FSS)UK (Strathclyde)Belgie (NICC)
Bart Nys May 2007
Survey - ConclusionA high demand exists for a GSR database, but very few labs canafford the necessary time to contribute in developing it.
The database would contain predominantly SEM data
Only half of the labs is sufficiently equipped to participate actively in adatabase development.
Management support is probably not very large (cost)
Form a Committee with a limited number of labsShare the results with the others
Bart Nys May 2007
ENFS1 Partners
" Austria" Deutschland (BKA)" Deutschland (LKA Sachsen-Anhalt)" Deutschland (LKA Berlin)" Espana" Espana" Finland" France" Greece" Israel" Italy" Lithuania
NetherlandsN-IrelandPoland
PortugalSchweiz (Zurich)Schweiz (St. Gallen)SlovakiaSuisse (ECRA)SwedenUK (FSS)UK (Strathclyde)Belgium (N ICC)
Bart Nys May 2007
GSR DatabaseThe "Database Gunshot Residues" Project
Official ENFSI Project started in 2000:
Project leader: Bait Nys - NICC
Project Coach:
Ludwig Niewoehner - BKA
Planning and Objectives:- Form a pilot group of forensic labs
(Belgium, Germany, Finland)- Develop database engine specific for GSR data- Compile common database of SEM data- Expand to other techniques (organic analysis methods)- Share the results with the international forensic community
Bart Nys May 2007
Database SpecificationGeneral Requirements:
"Independent of hardware platform (e.g. Byte ordering)
"Independent of software base (e.g. Operating System, Database)
" Small footprint data, easy to access and transmit" Standardised file formats, processable by a maximum of different
software packages" Common access method for internal and external users" User access Security" Access control to specific parts of the database
- Solution: System must be Internet-compliant
Bart Nys May 2007
Gunshot Residue Database
" "What type of ammunition is this?"" "Is the ammunition used in this case the same as in
this other case?"" "Was this type of particle ever seen in GSR samples
before?"
Catalogue of ammunition
* Development of new processing methods
Bart Nys May 2007
Correlation between analysis methods
Database SpecificationAdditional Project Features:
"European project, sponsored by AGIS funding : JAI/2003/AGIS/033 andJLS/2005/AG IS103 I
" PhD. at the University of Freiberg (Germany)." Development of Chemometric methods (based on Partial Least
Squares models) provides for Application-specific models used as asearch engine.
"Spectra used to build the models are stored on the server and can beconsulted as a reference.
" Database infrastructure is ready for future Applications eg. fingerprintingof primer compositions, morphological studies, combination of organicdata in the search......
" Server system installed at the Department of Justice Belgium." Operational test phase since March 2007." Will be officially presented to ENFSI in September 2007.
Bart Nys May 2007
7\ GSR Database Project
Home About Us Partners Reports Manuals Downloads Planning Links Site Map
These are the contributing Partners in the ProjectNeden ands Forensisch Insti tout
Arno, NkOdFtcut. Loan san Ypenburg 6 -2497 GB Den Haag -The Netherlands
Contact persons Amalia Brouwer-Stamouli and Jan Sieostraaten
K123 - Thaerstnasse 11 -65173 Wiesbaden - Deutschland
Contact persons" LuciwieNioeoehner and Martin Barth
Aita. I BunrJeskriminalamt
Reterat 1K -22-I -ELI-getorderte ProjekteAm Treptoser Park 5-0 - 12435 Berlin - Deutsohiand
Contact person Asia Nimke
Nationaallnatituutvoor Cnirninalistiek en Criminologie
Ins titut National de Cniminalistique et de CniminologiePEEP
Vilsoordsesteen'seg 100 -1120 Brussel - BelgiC
S Contact person - Cart NvsNC iiInstitute of Forensic Research in Cracow
Westerplatte St 9 -31 -033
Cracow - Poland
Contact person Zuzanna Brozek-Mucha
KA
<--09)-C) 'cj'
eQr r5
Li TECHNISCI-IF -
p UNIVERSITAT
6I B
KELJ FLCriminalistic Instituteaklabinska 1 -51272 Bratislasa -Slovak Republic
contact person Ronald Horvath
Institut fur nalytische ChemieLoipzigor Str 29- '99599 Freiborg
- Doutschland
Contact persons-Sylvia Stetten and Matthias Otto
AGIS project JAI 2003-AGIS-O3S
under the supervision of the ENFSI Expert Working Group Firearms
CopyrightOr 2006-2007 byDart Nvs -Last updated December2006
Bart Nys May 2007
Non-GSR Applications
" Paint Analysis (Car Paint Database)" Glass Characterisation"Light Bulb Filaments
" Unknown Material Analysis" Document Analysis (<<crossing line problem)))" Diatoms"Entymology
?? Killer Application??
Bart Nys May 2007
aqoLOOZJthJAI
0I0
VA
:Sk4k.
9p
SXMPEEl
Iv
N
0
!S
SISAleuvJuawel!d
Filament Analysis
r-10
Advantages of SEM/EDX:" Magnification
\" Depth of Field" BSE Imaging identifies Glass Fragments easily" X-ray Analysis confirms Fragment and Deposition Composition
Bart Nys May 2007
aqoLOOZJthJAI
S!sAleuvJuawel!d
SXMPEEl
Filament Analysis" Breaking of a cold filament
_____" Breaking of a lit filament
JfJJI
Breaking of a warm filamentgirn1d
()subsequently lighting it
" Breaking of a cold filament,
" Breaking of a cold filament,without breaking the bulb
" Breaking of a warm filament,without breaking the bulb
Using new and relatively new filaments (max. 20 hours of use)
Using worne filaments (lifetime unknown)
A total of fifty filaments were tested using both light macroscopy and SEM / EDX
Bart Nys May 2007
Filament AnalysisCase 1: Breaking of the Bulb of a lit Filament
Filament breaks after 2-3 seconds
Yellow deposit is formed
Sometimes small deformations
Overview
=> Use of the light macroscope
Glass Fragments Droplet-shaped Fracture
Bart Nys May 2007
V
Filament AnalysisCase 1: Breaking of the Bulb of a lit Filament
Filament breaks after 2-3 seconds
Yellow deposit is formed
=> Use of the SEM
Sometimes small deformations
Bart Nys May 2007
Overview Glass Fragment Droplet-shaped Fracture
Filament AnalysisBreaking of Light Bulbs without damage to the lit Filament:
Glass Fragments
Confirmation of Glass Fragment Composition using EDX Analysis:cps
1000
500
0keV
Bart Nys May 2007
0 2 4 6
8
Filament AnalysisBreaking of Light Bulbs without damage to the lit Filament:
Glass Fragments
Note: I in 4 Tests produced no Glass Fragments - after a light shock.
Bart Nys May 2007
aqoLOOZ'J'\I
A6ooqdowin6usiioivs3JoqdsoqsAws1uow6Jd
.JIq
wflog
vs6u!snpu!401Asoais1uow6Jdiods01PH
s/cMpug
S!sAleuvJuawel!d
Filament Analysis
Fracture morphology studied by SEM
Dprn
Cold Fracture
Bart Nys May 2007 be
Warm Fracture
Fracture in Air
Filament AnalysisFilament surface morphology studied by SEM
2OIir INew Filament
2Oprn
Used Filament showing 'staircases'
Young Filament (18 hours)
\ 1Orn
Worne Filament, oxidised
.,4Wt
Bart Nys May 2007
aqoLOOZJthJAI
.t
afl
:t'st:si
-
I"
4?
--'"" 00Hitt'r-:
-"-,
s!sAleuVjuawnoo(]
SXMPEEl
U
U
I--1
.SQCl)>CoC
is
CE000
rc
.?
rcA
"
F"F
'1
..
..
thI
"1-
".'
.:
tPLt
.:;!t-')
1
-La
IsCCNct[ID
k
I