Ambient Pressure Mass Spectrometry at the Sub Micron Scale

Lead Research Organisation: University of Surrey
Department Name: ATI Electronics

Abstract

This proposal aims to develop a new ambient pressure mass spectrometry imaging system. It will use a beam of ions accelerated to MeV potential energy - velocities of the order of 5% the speed of light or less. The beam will be focussed using a set of quadrapole magnetic lenses to less than a micron in size and will be passed out of the vacuum system through a 100nm thick silicon nitride window into air where it will be able to travel between 0.5-1.0cm before stopping. A sample placed in front of this beam of ions will be sputtered (eroded) by the interaction of the ions with the electrons in the system (electronic energy loss). Previous experiments in vacuum have demonstrated that if the sample is a molecular material it is possible to extract large (~45kDa) molecular species from the surface and that these can be detected in a Time of Flight mass spectrometer to determine their molecular mass. Fragments that are removed at the same time give indications about the bonding arrangements of the molecules sputtered and can be used to determine the probable molecular arrangement.
The beam itself can be raster scanned using an electrostatic field so that a molecular map of the surface of the material can be determined at the micron scale. The ions as they enter the surface of the material are moving fast enough that they will also cause electrons in the outer shells of the atoms that they pass to become exited and in relaxing back will give out a characteristic X-ray. These X-rays can also be collected and analysed using a technique known as Partical Induced X-ray Emmision (PIXE) to give trace element maps as well.
This will be the worlds first scanning mass spectrometer capable of imaging at the sub micron scale in air.
Applications for this equipment range from forensics to biomedicine taking in geology and the environment as well as helping to understand the origins and manufacture of art and archeological remains. These applications will be encouraged over the period of the project.

Planned Impact

This application is to construct the worlds first scanning ambient pressure secondary ion mass spectrometry system with sub micron resolution. It has impact across a number of disciplines of which we have identified 4 key areas to target during the grant period. These are forensics science, biomedicine, archaeometry and geology and the environment.

The initial impact will be to the accademic researchers who will be able to gain access to the equipment many of which have submitted letters of support with this application. The companies supplying the equipment required to manufacture this instrument are UK based and will be in a good position to exploit an expected market in new instruments like these. The market wil not be huge, maybe 10 or 20 such machines.

The subsequent impact of the research that this equiment will enable is potentially huge:
Informing pharmeceutical companies and the NHS on precisely how drugs are reacting with living systems such as cells. This will allow drugs to be designed with more precision and understanding so that side-effects may be minimised and the primary aim maximised. A number of cancer related drugs and activities have been highlighted as of interest to the Addenbrooke's Hospital in Cambridge as part of an on-going collaboration.
Work in forensics science aimed at extracting more information from fingerprints - with in air analysis this could even be performed covertly - has impact in helping to identify criminals even with only smudged prints. Other aspects of forensic science include providing quartz grain analysis for identification of soils which will provide substantial support for the current texture analysis. The analysis of gun shot residues for organic species will help identify new non-lead bearing ammunition residues.
Molecular analysis of parchments can only really be done in air - it is not normally considered acceptable to takes samples from ancient relics or, often, to place them in a vacuum system. The molecular analysis of the parchment material can yield surprising information about the origins of the material and, as the parchment is often orgainc in nature and the product often of an agricultural community, can reveal aspect of community life. Other aspects here include anlysis of paint binders for provenancing, normally the trace element ratios are employed, but the binders are again often natural organic materials which may well be more informative about origins than just the trace elements.
The Goeology and Environment has impact in studies of small inclusions locked up for thousands of years in geological samples. The information in these inclusions can reveal past climate and atmospheric changes on a geological scale. The environmental issues relating to bioremediation and airborne particulates have high potential impact in both providing a method to clean up polluted sites and one for monitoring airborne pollution.

Publications

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Jeynes C (2012) "Total IBA" - Where are we? in Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms

 
Description A new Ambient pressure imaging mass spectrometry system has been developed. This AP-MeV_SIMS system has gradually come on-line, slower than originally planned, due unforeseen difficulties with background molecular signals from the ambient as well as low pick-up of the signal from the target due to unexpected issues of gas dynamics immediately around the target area. These issues have been informed by substantial modelling, which has improved the signal to noise ratio by several orders of magnitude. But still much work needs to be done to make this a truly valuable technique.

As a side issue AP-MS was initiated in the detection of drugs of abuse in fingerprints. It was found that not just the drug but also its metabolites are readily detected in drug users fingerprints, demonstrating for the first time that someone has not only handled a drug but also ingested it. This created a lot of interest in the media world wide with over 500 media hits.

Development of the ambient technique continues some limited images have been achieved, but the airborne nature of some materials can make imaging difficult. For example a pellet containing traces of caffeine and cocaine was imaged and while the cocaine was observed in the pellet, the caffeine was found in the gas phase all around the pellet, limiting the ability of the technique to locate the origin of the molecule.
Exploitation Route The equipment still has a large number of potential users and as the instrument improves we will work with users to produce new uses of the instrument. The Coordinated Research Project (CRP) of the IAEA brings together a group of people across the world developing this kind of instrument.
Publications are in the pipeline for the use and development of the instrument.
Sectors Aerospace, Defence and Marine,Agriculture, Food and Drink,Chemicals,Electronics,Energy,Environment,Healthcare,Leisure Activities, including Sports, Recreation and Tourism,Manufacturing, including Industrial Biotechology,Culture, Heritage, Museums and Collections,Pharmaceuticals and Medical Biotechnology,Security and Diplomacy

 
Description We have initiated a Co-ordinated Research Project (CRP) at the International Atomic Energy Agency (IAEA) to develop the use of MeV SIMS in other UN countries. Since we started this project groups in Croatia, Slovenia, Brazil, Germany, Italy and Switzerland have started to set up similar facilities to those at Surrey. Surrey has been key to developing new training initiatives with the IAEA on the use of MeV SIMS. MeV SIMS has become a key component in a work package of a MCITN run from Surrey.A further Application to EPSRC for a combined DAPNE IBA analysis system has been successful and the integration with joint programmes with NPL in mass spec analysis has resulted in two new PhDs and one of the Surrey team now working full time at NPL. There are now 6 MeV-SIMS installations around the world, in Germany, Switzerland, Japan, Slovenia, Croatia and here. Only two f these have attempted ambient pressure analysis. We have obtained time at the AGOR facility in Groningen to use their GeV ion beam with our mass spectrometer to explore the use of such beams for SIMS. We expect to be able to use this beam to substantially increase the yield of large molecular species in full ambient. This has the potential to lead to a new variant of the technique.
First Year Of Impact 2016
Sector Aerospace, Defence and Marine,Chemicals,Energy,Environment,Healthcare,Culture, Heritage, Museums and Collections,Security and Diplomacy
Impact Types Societal,Economic

 
Description EU FP7 MCITN
Amount £1,800,000 (GBP)
Funding ID 317169 
Organisation European Commission 
Department Seventh Framework Programme (FP7)
Sector Public
Country European Union (EU)
Start 01/2013 
End 12/2016
 
Description FP7 Integrated Infrastructures Initiative (I3)
Amount € 1,176,245 (EUR)
Funding ID 227012 
Organisation European Commission 
Department Seventh Framework Programme (FP7)
Sector Public
Country European Union (EU)
Start 02/2009 
End 02/2013
 
Description Impact Acceleration Account - BP
Amount £20,000 (GBP)
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Academic/University
Country United Kingdom
Start 07/2013 
End 07/2014
 
Description Impact Acceleration Account - Intelligent Fingerprinting Ltd
Amount £20,000 (GBP)
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Academic/University
Country United Kingdom
Start 05/2013 
End 07/2014
 
Description Kyoto 
Organisation University of Kyoto
Country Japan 
Sector Academic/University 
PI Contribution Collaboration in setting up a vacuum MeV SIMS system. The group at Kyoto provided us with several hardware items and initial technological support
Collaborator Contribution We provided our expertise in microbeams and imaging. Interfacing our equipment with theirs to provide an enhanced imaging capability.
Impact Papers and joint talks at conferences as well as technical meetings at the IAEA in Vienna and the creation of a Coordinated Research project on MeV-SIMS and Heavy Ion PIXE
Start Year 2016
 
Description ALD Finland CoE Scientific Advisory Panel 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Scientific Advisory Panel of the Finland Centre of Excellence for Atomic Layer Deposition. Part of this was the use of ion beam analysis to characterise the ALD films grown. Opportunity to demonstrate use of high accuracy IBA and molecular analysis techniques to audience of ALD practitioners and industrial partners
Year(s) Of Engagement Activity 2017
 
Description IAEA Consultant Meeting 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Part of a small consultant panel to determine how to setup and run a "Roadmap for Ion Beam Technologies". A survey of the community was conducted and advertised at a number of international conferences, as well as a workshop at the International Conference on Ion Beam Analysis in Croatia this year. A second workshop will be held at the International Conference on Ion Beam Modification of Materials in New Zealand in 2016 to include this aspect into the roadmap. The Roadmap is to be held on the accelerator portal of the IAEA website.
Year(s) Of Engagement Activity 2015
URL https://nucleus.iaea.org/sites/accelerators/IBT_Roadmap/SitePages/Home.aspx
 
Description ICTP-IAEA Advanced Workshop on High Sensitivity 2d & 3D Characterisation and Imaging with Ion Beams 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Co-director of an advanced training course organised at the ICTP in Trieste with the IAEA in Vienna. $ guest lecturers from labs in Brazil, Portugal, France and the UK provided lectures and training material for the workshop. The course was limited to 30 participants from around the world part sponsored by the IAEA. The workshop involved discussions on the application of ion beams for analysis and the use of MeV-SIMS.
Year(s) Of Engagement Activity 2016
URL http://indico.ictp.it/event/7638/
 
Description UK National Ion Beam Centre open day 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Professional Practitioners
Results and Impact Open Day to bring together existing, new and prospective users of the UK National Ion Beam Centre. Opportunity to talk to people about the facilities availabel and abou th enew facilities coming on line as a result of some of the capital equipment grants awarded by EPSRC.
Year(s) Of Engagement Activity 2017