forensic applications of sem/edx, p-xrf and xrd at the national...

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

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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

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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

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" 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

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Zone 1

Benchtop

Zone 2010F- R2

R3 Zone i

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RI

Zone 2

Labs

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Bart Nys May 2007

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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

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Gunshot Residue Application

Deposition

Sides

Shooter

Hands

Clothing

Face - Hair (rifle)

Shooting Environment

uzzle

Target

Clothing

Objects in Vicinity

Bart Nys May 2007

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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

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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

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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

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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

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Filament Analysis

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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

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Filament Analysis" Breaking of a cold filament

_____" Breaking of a lit filament

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Breaking of a warm filamentgirn1d

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" 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

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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

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Bart Nys May 2007

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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

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Filament Analysis

Fracture morphology studied by SEM

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Warm Fracture

Fracture in Air

Filament AnalysisFilament surface morphology studied by SEM

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