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Final Report Summary - ROSFEN (Rapid On-site Forensic Analysis of Explosives and Narcotics)

Executive Summary:
The aim of the ROSFEN project was to deliver an advanced forensic platform for rapid, on-site direct detection and lab-quality analysis of explosives and their precursors. The ROSFEN platform developed during the project is designed to be a tool for sample collection, with on-site detection, screening and analysis of explosives with sensitivity and selectively comparable to state of the art laboratory instrument.

Technological innovation is combined with development of best practice protocols for evidence collection and data management to preserve chain of evidence from the site to the trial. During the project, the project partners have successfully demonstrated:

• Development of novel receptor molecules tailored for selective adsorption of specific explosive compounds to enable pre-concentration prior to thermal desorption and analysis.

• Demonstration of selectively binding of explosive analytes, with controlled thermally-induced release, in excellent agreement with computational modelling results.

• Development of a compact system based on novel ion filtering, including all necessary components, sub-systems and bespoke graphical user interface. Identification of test compounds, analytes and interferant is achieved by a miniaturised solid state quadruple MS detector .

• Detection of different classes of explosives analyte vapours with limits of detection ≤1 ng/mL, achieving the main project technical target.

• Successful demonstration of the ROSFEN platform to representative from civilian police forces and forensic laboratories from a number of EC states.

A public website has also been established at in order to publicise the goals of the project, introduce the consortium and disseminate progress to the wider scientific community, industry and the public. Details on publications and presentations are available on the project web site; a project flyer summarising the project details and results will be available for download shortly.

Project Context and Objectives:
Ensuring the safety and security of Europe’s citizens and infrastructure remains a significant challenge. Europe faces a rising threat from terrorist attacks using improvised explosive devices (IEDs), including under-vehicle, command wire, vehicle-borne and projectiles. Forensic analysis is an essential resource in the battle against organised crime and terrorist attacks. A key challenge in forensics is the detection of trace explosive residues at a post-blast scene or on the hands or clothes of an alleged suspect. Explosives include nitroaromatics (e.g. DNT, TNT), nitro-amines (e.g. RDX), nitro-esters (e.g. PETN) and organic peroxides (e.g. TATP). Detection of explosives requires that a response, such as the binding or ionisation of the trace compound, leads to a sensor output, such as a signal change.

The challenge of developing a universal sensor for explosives arises from the diverse characteristics of the analytes, including vapour pressure, volatility, polarity and solubility, as well as molecular weight and structure. Other sensing methods such as IMS, dogs, X-ray dispersion and chemical fluorescence have limitations that may introduce false negative results due to chemical interferents and contamination, or false positives from compounds with similar physical properties.

As a result, the current challenges in detection and analysis of explosive materials, drugs and precursor materials relate to:

• Sensitivity, a very low limit of detection is usually required to detect materials with low volatility.

• Selectivity and false alarm rate. In particular, chemical interferents can "mask" the presence of the chemical species of interest.

• Speed or ‘response time’, including data processing, sample clean-up or separation.

ROSFEN’s goal was therefore to deliver an advanced forensic platform for rapid, on-site direct detection and lab-quality analysis of explosives and their precursors. The ROSFEN platform is a tool for sample collection, on-site detection, screening and analysis of explosives, together with development of best practice protocols for evidence collection and data management to preserve chain of evidence from the site to the trial. The project objectives were:

• Development of novel molecular materials for selective adsorption of specific explosive compounds to enable pre-concentration prior to thermal desorption and analysis.

• Development of a compact, field-deployable system based on novel ion filtering, coupled with identification by a miniaturised tandem mass spectrometer (MS-MS).

• Adherence to best practice for evidence collection and best practice protocols for forensic analysis.

• Detection of explosives and their chemical precursors with limits of detection ≤1 ng/mL.

• Response times (from sample insertion to result and analysis) of < 10 seconds.

• High selectivity, resistance to false negative results due to chemical interferents and false positives caused by compounds with similar physical properties.

Project Results:
Tyndall-UCC studied the binding of pentaerythritol tetranitrate (PETN) with the receptor molecules designed and synthesised by UNIBAS using density functional theory (DFT). ab initio simulations confirmed that the nitrate groups in PETN interact with the uracil recognition groups in the receptors by hydrogen bonding. Dynamical liquid state models showed PETN is well bound to receptors in the IPA solvent (used for swab sample collection) when the temperature is increased up to 400 K. The calculations predicted that the PETN would be successfully desorbed (released) from the receptor, when the temperature is increased to 500 K.

The development and optimisation of the sample heating module and on the sub-components (such as molecular binding traps for PETN and high surface area templates) for the analyte concentrator module was successfully completed. The sample introduction module developed by Environics worked well in tests and desorption of PETN from swab material was demonstrated.

UNIBAS designed and synthesised a series of fluorescent receptor molecules. These molecular traps covalently bind to anodised aluminium oxide (AAO) high surface area template substrates developed by Tyndall-UCC and can be used to trap (and thermally release) PETN. In situ PETN exposure testing by Tyndall-UCC shows a reduction in fluorescence intensity following PETN exposure (consistent with PETN binding) and a subsequent increase in fluorescence intensity following thermal annealing at 150 oC (423 K), in close agreement with calculations.

Environics, with assistance from Microsaic, led the integration and demonstration of a breadboard ion filtered MS. The sample introduction and ion filter modules were coupled to a SESI source and a Single-Quad MS. Performance testing was undertaken with this breadboard system. An ion optics assembly has been designed and constructed. Microsaic has investigated the optimum geometry and experimental setup for SESI using its MEMS electrospray source as the source of reagent ions. A Single-Quad MS was used instead of Triple-Quad MS as the platform for testing of the SESI/ion filter.

This allowed the Triple-Quad and SESI/ion filter development programmes to run in parallel. Environics has been testing the performance of the breadboard ion-filter MS with known samples of PETN and provided support for FSNI to evaluate the system. A complete prototype comprising a heated sample introduction module, an ion filter with an integrated SESI source, and a miniature Single-Quad MS has been demonstrated and extensively characterised. Microsaic has developed a miniature Triple-Quad MS breadboard based on its MEMS mass spectrometry components.

The integration of all the components i.e. sample introduction and concentrator modules, the DMS ion-filter, the SESI source (using the Microsaic ESI spray pen); the Vac chip and the concentrator were completed by Environics. Miniaturisation has been achieved through the use of chip-scale components: these were integrated with the Microsaic Single-Quad MS detector. It has been demonstrated that PETN can be vaporised in the sample chamber and detected by contact with the charging spray by secondary ionisation. Limit of detection obtained using the liquid headspace chamber was 10 ng, matching the main project technical objective.

Microsaic have also carried out the development of a new Triple-Quad detector, with improved sensitivity and selectivity, equipped with a single overarching control system operating the three quadrupoles, based on modifications to their existing technology. Microsaic are now developing a compact module for testing in the tandem MS prototype.

Testing of the performance of the completed prototype was carried out by FSNI, in conjunction with PSNI, based on the detailed validation plan developed during the second half of the project. Dissemination was mainly done through the poster sessions in three different international forensic conference and one ion spectrometry conference. Presentation of the completed tandem MS system at a dedicated end users workshop was successful, the ROSFEN platform being seen as useful equipment to complement current offering in explosives and narcotics identification.

Exploitation of the project results will be mostly utilization of the sub-systems developed in the project. In addition, essential (secret) know-how and technical knowledge of the forensic process has been increased for all partners, especially in the companies. These initial tests have shown that analysis of PETN can be achieved using the head space sample chamber and the SESI source on the breadboard of the ROSFEN instrument: the potential for a sensitive system for detection of PETN was demonstrated.

Exploitation of Foreground

As the ROSFEN platform is still at an early technical readiness (TRL) level, commercial utilization of the end product will not be possible without further development. However, the components and sub-systems are available for future commercial exploitation. The status at the end of the project was as follows:

The sample introduction module:

• Development of the sample introduction module has improved greatly Environics’ know-how of sample extraction and solid sample handling. The training provided by PSNI to Environics Oy’s personnel has provided also insight of the topic and had impact to completely different domain in Environics Oy: some design and production practises Environics Oy have been improved based on this insight.

• Knowledge and design of the solid sample handling can be utilized in the applications related to Environics traditional CBRN business.

• The complementary concentrator module was developed at the end of the project and still requires further testing and evaluation before exploiting.

Differential mobility spectroscopy (DMS):

• Development of DMS required several design and development cycles, which revealed a lot of things that were unknown for developing engineers. During these design cycles, Environics and its engineers have gained a lot of new knowledge related to high-voltage high-speed signal processing environment, design against EMC and EMI issues and some manufacturing techniques.

• Development results and know-how has been utilized in new industrial analyser prototype development

DMS driver:

• As for the DMS unit, several development cycles and result can be used in future products with small modifications. Special understanding of switched HV-circuit design was gained.

• Utilization has already been started with analyser prototype and also other R&D


• Software development has created platform and ideas for sw-development in commercial product.

• Software development also lead to scalable UI platform: the system can be used in simple small card-type computers and also in full scale PCs.

Potential Impact:
ROSFEN’s goal was to deliver a platform for on-site forensic analysis of explosives, narcotics and other precursor materials by generation of laboratory-quality data at crime scenes, enhancing forensic-led policing and improving conviction rates and undermining paramilitary campaigns. The ROSFEN project has delivered an innovative platform for on-site forensic analysis by combining technology from two research-led SME: ion mobility spectrometry (IMS) technology from (Environics, FI) with chip-based tandem mass (MS) spectrometry (Microsaic System, UK).

ROSFEN integrates IMS with tandem MS into a micro-engineered platform as the basis of a field portable analytical technology capable of positive identification of explosives and chemical precursors by filtering out chemical noise from interferents (e.g. fuel oils, masking agents), and isolating the chemical isomers of interest.

ROSFEN has been driven by first responder and end user requirements to provide rapid screening and positive identification with detection levels < 10 ng/ ml. To address these challenges, ROSFEN partners developed new scientific knowledge, in areas ranging from thermal desorption and secondary electrospray ionisation of samples to field asymmetric ion mobility (FAIMS) and ion optics, to produce an advanced forensic platform. Common sample collection & pre-concentration protocols, sample heating and sample introduction technologies and multipass sample recycling to increase detected analyte fraction will be developed and maintained across all platforms.

One of the impacts of the project will be a substantially strengthened global competitiveness of European industry in Security. This will be achieved using ion filtering technology to couple with next-generation micro-analytical devices into a powerful, multi-sensing tool capable of identifying trace quantities of the chemical species of interest in complex matrices such as environmental samples.

Today, there are no truly portable, compact or affordable MS products suitable for these applications. Integration of key MS components using MEMS technology has the potential to transform the size and cost of MS systems and allow of MS to be used not only in forensic laboratories, but also by community and national reference laboratories, hospitals, etc.

The core technology concept, ion filter tandem MS, has applications in several market segments, and could generate multiple revenue streams. Longer term, this technology can be further developed to analyse medicines, food, feed and drink for prohibited substances, and potentially to analyse body fluids and tissue in oncology laboratories, and also in field for screening of food, feed and animal medicine.

The new portable, ion filer tandem MS platform developed within the project will boost the innovation union and the competitiveness of European industry in the MS market. The tandem MS platform is intended for application within the MS industry, estimated at $3.3B worldwide, and in particular the $2.0B security market, and the $44M portable MS segment.

Through the intensive cooperation between internationally renowned end-users and two high tech SMEs planned in the project, the ROSFEN partners seek to bridge the gap between research and market. The consortium aims to exploit the platform through co-marketing to their customers and partners, while research actions around standards and interoperability accelerate adoption of the platform by the European security market.

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