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Dr Vladimir Palitsin


Laboratory Manager
PhD
+44 (0)1483 682243

Biography

Biography

Vladimir joined the Surrey Ion Beam Center (IBC) as a Research Fellow in March 2006 to work on development of the new nanobeam facilities, the Horizontal Nanobeam and the Vertical Nanobeam.

He holds MSc in Physical Electronics from Tashkent Technical University (1985) and PhD in Physics from the University of Warwick (2006). During PhD work in the group of Professor Mark Dowsett he was engaged in development of MEIS/SIMS for surface and thin film analysis and in the evaluation of the ultra low energy SIMS (uleSIMS) as a mass spectroscopic technique in the applications to archaeometry and cultural heritage.

Before this he worked as a scientific researcher at Arifov Institute of Electronics, Uzbek Academy of Sciences (1985-2000), and as a visiting researcher in the I.U.T. Berlin (1997-2000) and the University of Antwerp (2000-2002).

Some of his earlier projects include development of the Ion Mobility Spectrometers and detectors for forensic and environmental trace analysis, ion sources for mass spectrometry and detectors for the gas chromatography. During that time he has also gained an extensive practical knowledge of SIMS as well as MEIS, SEM and XPS techniques.

The primary objectives of his current research are development of the novel analytical techniques in the IBC. These include the ambient pressure MeV energy mass spectrometry (MeV SIMS) with (sub)-micron resolution, and application of proton (ion) beam writing (PBW) technologies for 3D-micromachining of high aspect ratio microstructures: lab-on-a-chip, neural biosensors, micro-fluidics devices, micro-actuators.

Research interests

  • development of analytical instrumentation, systems engineering
  • mass spectrometry and imaging mass spectroscopy
  • ion beam applications for material analysis and material modification
  • charged particle optics
  • microfabrication using ion beam technique

My publications

Publications

Al-Shehri S, Palitsin V, Webb RP, Grime GW (2015) Fabrication of three-dimensional SU-8 microchannels by proton beam writing for microfluidics applications: Fluid flow characterisation, NUCLEAR INSTRUMENTS & METHODS IN PHYSICS RESEARCH SECTION B-BEAM INTERACTIONS WITH MATERIALS AND ATOMS 348 pp. 223-228 ELSEVIER SCIENCE BV
Al-Shehri S, Palitsin V, Webb RP, Grime GW (2015) Fabrication of three-dimensional SU-8 microchannels by proton beam writing for microfluidics applications: Fluid flow characterisation, Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 348 pp. 223-228
The proton beam writing (PBW) technique was used to fabricate microfluidic structures in SU-8 resist. A network of the buried channels was fabricated as part of a project to develop functional microfluidic device for neuronal studies and self-powered microfluidics. Protons with energies between 2.5 MeV and 0.75 MeV were used to fabricate the buried channels with a minimum feature size of around 1 ¼m and depths of 40?55 ¼m. Roughness of channels sidewalls was around 2.5 nm rms. Exposure regime and examples of functional networks fabricated using PBW are described. COMSOL Multiphysics® software was used to model the flow characteristics of fluid in the SU-8 microchannels structured by PBW. The results obtained using PBW are compared with the structures fabricated by UV-lithography.
Belykh SF, Palitsin V, Veryovkin IV, Kovarsky AP, Chang RJH, Adriaens A, Dowsett M, Adams F (2006) Caesium sputter ion source compatible with commercial SIMS instruments, APPLIED SURFACE SCIENCE 252 (19) pp. 7321-7325 ELSEVIER SCIENCE BV
Jones BN, Palitsin V, Webb R (2010) Surface analysis with high energy time-of-flight secondary ion mass spectrometry measured in parallel with PIXE and RBS, NUCLEAR INSTRUMENTS & METHODS IN PHYSICS RESEARCH SECTION B-BEAM INTERACTIONS WITH MATERIALS AND ATOMS 268 (11-12) pp. 1714-1717 ELSEVIER SCIENCE BV
Merchant M J, Jeynes JCJ, Grime GW, Palitsin V, Tullis IDC, Barber P, Vojnovic B, Webb RP, Kirkby KJ (2012) A focused scanning vertical beam for charged particle irradiation of living cells with single counted particles, Radiation Research: an international journal forthcoming Radiation Research Society
The Surrey vertical beam is a new facility for targeted irradiation of cells
in medium with singly counted ions. A duo-plasmatron ion source and a 2
MV Tandem accelerator supply a range of ions from protons to calcium for
this beamline, with energy ranges from 0.5 to 12 MeV. A magnetic quadrupole
triplet lens is used to focus the beam of ions. We present the design of this
beamline, and early results showing the capability to count single ions with
98% certainty on CR-39 track etch. We also show that the beam targeting
accuracy is within 5 microns and selectively target human broblasts with a
H2AX immuno
uorescence to demonstrate which
cell nuclei were irradiated. We discuss future commissioning steps necessary to
achieve sub-micron targeting accuracy with this beamline.
Merchant MJ, Palitsin V, Grime GW (2009) The use of the Wien filter to eliminate object slit scattering in MeV ion nanobeam systems, NUCLEAR INSTRUMENTS & METHODS IN PHYSICS RESEARCH SECTION B-BEAM INTERACTIONS WITH MATERIALS AND ATOMS 267 (12-13) pp. 2021-2023 ELSEVIER SCIENCE BV
Sani SFA, Grime GW, Palitsin V, Mahdiraji GA, Rashid HAA, Maah MJ, Bradley DA (2015) Micro-PIXE analysis of doped SiO2 fibres intended as TL dosimeters for radiation measurements, X-RAY SPECTROMETRY 44 (2) pp. 33-40 WILEY-BLACKWELL
Belykh SF, Palitsin VV, Veryovkin IV, Kovarsky AP, Chang RJ, Adriaens A, Dowsett MG, Adams F (2007) New Cs sputter ion source with polyatomic ion beams for secondary ion mass spectrometry applications., Rev Sci Instrum 78 (8)
A simple design for a cesium sputter ion source compatible with vacuum and ion-optical systems as well as with electronics of the commercially available Cameca IMS-4f instrument is reported. This ion source has been tested with the cluster primary ions of Si(n)(-) and Cu(n)(-). Our experiments with surface characterization and depth profiling conducted to date demonstrate improvements of the analytical capabilities of the secondary ion mass spectrometry instrument due to the nonadditive enhancement of secondary ion emission and shorter ion ranges of polyatomic projectiles compared to atomic ones with the same impact energy.
de la Mata BG, Dowsett MG, Palitsin V (2005) Ultra-low energy SIMS study of ultra-shallow boron implants in HPHT diamond, PHYSICA STATUS SOLIDI A-APPLICATIONS AND MATERIALS SCIENCE 202 (11) pp. 2148-2153 WILEY-V C H VERLAG GMBH
Warmenhoven J, Demarche J, Palitsin V, Kirkby K, Webb P (2015) Modeling transport of secondary ion fragments into a mass spectrometer, Physics Procedia 66 pp. 352-360
The Surrey Ion Beam Centre was awarded the Engineering and Physical Sciences Research Council (EPSRC) grant for ?Promoting Cross Disciplinary Research: Engineering and Physical Sciences and Social Sciences? allowing continued research into the characteristics of desorption of secondary ions by the impact of fast primary ions in the ambient pressure at the sub-micron scale. To carry out this research a new beamline has been constructed consisting of a time-of-flight secondary ion mass spectrometer combined with the current 2MV Tandem accelerator. This research has already returned many significant results such as the first simultaneous SIMS, PIXE and RBS measurement preformed on an organic sample in vacuum. However, further optimization and validation of the new beamline is still being worked on. This work focuses on the optimization of the end station geometry to allow for high sensitivity ambient pressure measurements. It is concluded that a common geometry can be adopted for a wide variety of smooth samples to ensure optimum sensitivity provided a hard edge of the sample can be found to place the mass spectrometer capillary near.
Jeynes JC, Merchant MJ, Barazzuol L, Barry M, Guest D, Palitsin VV, Grime GW, Tullis ID, Barber PR, Vojnovic B, Kirkby KJ (2013) "Broadbeam" irradiation of mammalian cells using a vertical microbeam facility., Radiat Environ Biophys 52 (4) pp. 513-521
A "broadbeam" facility is demonstrated for the vertical microbeam at Surrey's Ion Beam Centre, validating the new technique used by Barazzuol et al. (Radiat Res 177:651-662, 2012). Here, droplets with a diameter of about 4 mm of 15,000 mammalian cells in suspension were pipetted onto defined locations on a 42-mm-diameter cell dish with each droplet individually irradiated in "broadbeam" mode with 2 MeV protons and 4 MeV alpha particles and assayed for clonogenicity. This method enables multiple experimental data points to be rapidly collected from the same cell dish. Initially, the Surrey vertical beamline was designed for the targeted irradiation of single cells with single counted ions. Here, the benefits of both targeted single-cell and broadbeam irradiations being available at the same facility are discussed: in particular, high-throughput cell irradiation experiments can be conducted on the same system as time-intensive focused-beam experiments with the added benefits of fluorescent microscopy, cell recognition and time-lapse capabilities. The limitations of the system based on a 2 MV tandem accelerator are also discussed, including the uncertainties associated with particle Poisson counting statistics, spread of linear energy transfer in the nucleus and a timed dose delivery. These uncertainties are calculated with Monte Carlo methods. An analysis of how this uncertainty affects relative biological effect measurements is made and discussed.
Palitsin VV, Dowsett MG, Mata BGDL, Oloff IW, Gibbons R (2006) uleSIMS characterization of silver reference surfaces, Applied Surface Science 252 (19) pp. 7132-7135
Ultra low energy SIMS (uleSIMS) is a high sensitivity analytical technique that is normally used for ultra shallow profiling at a depth resolution of up to1 nm. This work describes the use of uleSIMS as both a spectroscopic and depth-profiling tool for the characterization of the early stages of corrosion formed on reference surfaces of silver. These samples are being developed to help with the characterization of tarnished surfaces in a cultural heritage context, and uleSIMS enables the tarnishing to be studied from its very earliest stages due to its high sensitivity (ppm-ppb) and surface specificity. We show that, uleSIMS can be used effectively to study the surface chemistry and aid the development of reference surfaces themselves. In particular, handling contaminants, surface dust, and residues from polishing are relatively easy to identify allowing them to be separated from the parts of the mass spectrum specific to the early stages of corrosion. © 2006 Elsevier B.V. All rights reserved.
Merchant MJ, Grime GW, Palitsin V (2010) The influence of stray DC magnetic fields in MeV ion nanobeam systems, NUCLEAR INSTRUMENTS & METHODS IN PHYSICS RESEARCH SECTION B-BEAM INTERACTIONS WITH MATERIALS AND ATOMS 268 (11-12) pp. 1933-1937 ELSEVIER SCIENCE BV
Sani SFA, Mahdiraji GA, Shafiqah ASS, Grime GW, Palitsin V, Hinder SJ, Tamchek N, Rashid HAA, Maah MJ, Watts JF, Bradley DA (2015) XPS and PIXE Analysis of Doped Silica Fibre for Radiation Dosimetry, JOURNAL OF LIGHTWAVE TECHNOLOGY 33 (11) pp. 2268-2278 IEEE-INST ELECTRICAL ELECTRONICS ENGINEERS INC
The material characteristics of doped SiO2 fibre are studied, the electron traps in the product medium creating a situation attractive for their application in thermoluminescence (TL) radiation dosimetry. To date, rather limited research has been conducted towards gaining an essential understanding of the magnitude of TL signal and material characteristics of doped fibres. Characterization is being sought to ensure that the mechanism of TL yield in optical fibres is well understood, allowing a favourable well controlled production situation to be established. The intended end point is to specify dosimeters, not only for clinical dosimetry but also for their application in industrial/energy-industry settings. Investigation of the surface oxidation state of the Ge-doped SiO2 optical preform has been carried out using the X-ray photoelectron spectroscopy technique. In a further development using the fibre forming technology, particle-induced X-ray emission/Rutherford back scattering measurements have been employed to ascertain dopant concentrations of Ge-doped-cladding photonic crystal fibres (PCFs) with a view to improving TL yield. Present results concern uncollapsed and collapsed-hole-PCFs.
Antwis L, Browton M, Palitsin V (2014) Development of a fast acting vacuum isolation valve for use with ambient ion beam analysis techniques, Vacuum 99 pp. 26-27
The development of an ambient pressure MeV SIMS ion beam analysis capability at the Surrey Ion Beam Centre has necessitated the development of a system to protect the vacuum integrity of the main 2 MV tandem particle accelerator. The development and operating characteristics of a fast acting vacuum isolation valve based on the principle of an induction coil are reported and shown to be suitable for the intended application. © 2013 Elsevier Ltd. All rights reserved.
Jeynes C, Bailey MJ, Bright NJ, Christopher ME, Grime GW, Jones BN, Palitsin VV, Webb RP (2012) "total IBA" - Where are we?, Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms 271 pp. 107-118
The suite of techniques which are available with the small accelerators used for MeV ion beam analysis (IBA) range from broad beams, microbeams or external beams using the various particle and photon spectrometries (including RBS, EBS, ERD, STIM, PIXE, PIGE, NRA and their variants), to tomography and secondary particle spectrometries like MeV-SIMS. These can potentially yield almost everything there is to know about the 3-D elemental composition of types of samples that have always been hard to analyse, given the sensitivity and the spacial resolution of the techniques used. Molecular and chemical information is available in principle with, respectively, MeV-SIMS and high resolution PIXE. However, these techniques separately give only partial information - the secret of "Total IBA" is to find synergies between techniques used simultaneously which efficiently give extra information. We here review how far "Total IBA" can be considered already a reality, and what further needs to be done to realise its full potential. © 2011 Elsevier B.V. All rights reserved.
Jones B, Matsuo J, Nakata Y, Yamada H, Watts J, Hinder S, Palitsin V, Webb R (2010) Comparison of MeV monomer ion and keV cluster ToF-SIMS, Surface and Interface Analysis Wiley Interscience
Palitsin V, Jeynes J, Jeynes C, Townley H (2016) Direct quantification of rare earth doped titania nanoparticles in individual human cells, Nanotechnology 27 (28) Institute of Physics
There are many possible biomedical applications for titania nanoparticles (NPs) doped with rare earth elements (REEs), from dose enhancement and diagnostic imaging in radiotherapy, to biosensing. However, there are concerns that the NPs could disintegrate in the body thus releasing toxic REE ions to undesired locations. As a first step, we investigate how accurately the Ti/REE ratio from the NPs can be measured inside human cells. A quantitative analysis of whole, unsectioned, individual human cells was performed using proton microprobe elemental microscopy. This method is unique in being able to quantitatively analyse all the elements in an unsectioned individual cell with micron resolution, while also scanning large fields of view. We compared the Ti/REE signal inside cells to NPs that were outside the cells, non-specifically absorbed onto the polypropylene substrate. We show that the REE signal in individual cells co-localises with the titanium signal, indicating that the NPs have remained intact. Within the uncertainty of the measurement, there is no difference between the Ti/REE ratio inside and outside the cells. Interestingly, we also show that there is considerable variation in the uptake of the NPs from cell-to-cell, by a factor of more than 10. We conclude that the NPs enter the cells and remain intact. The large heterogeneity in NP concentrations from cell-to-cell should be considered if they are to be used therapeutically.
Costa Catia, Webb Roger, Palitsin Vladimir, Ismail Mahado, de Puit Marcel, Atkinson Samuel, Bailey Melanie (2017) Rapid, secure drug testing using fingerprint development and paper spray mass spectrometry, Clinical Chemistry 63 (11) pp. 1745-1752 American Association for Clinical Chemistry

BACKGROUND: Paper spray mass spectrometry6 is a technique
that has recently emerged and has shown excellent
analytical sensitivity to a number of drugs in blood. As an
alternative to blood, fingerprints have been shown to
provide a noninvasive and traceable sampling matrix.
Our goal was to validate the use of fingerprint samples to
detect cocaine use.

METHODS: Samples were collected on triangular pieces
(168 mm2) of washed Whatman Grade I chromatography
paper. Following application of internal standard,
spray solvent and a voltage were applied to the paper
before mass spectrometry detection. A fingerprint visualization
step was incorporated into the analysis procedure
by addition of silver nitrate solution and exposing the
sample to ultraviolet light.

RESULTS: Limits of detection for cocaine, benzoylecgonine,
and methylecgonine were 1, 2, and 31 ng/mL respectively,
with relative standard deviations of less than 33%. No
matrix effects were observed. Analysis of 239 fingerprint
samples yielded a 99% true-positive rate and a 2.5%
false-positive rate, based on the detection of cocaine,
benzoylecgonine, or methylecgonine with use of a single
fingerprint.

CONCLUSIONS: The method offers a qualitative and noninvasive
screening test for cocaine use. The analysis
method developed is rapid (4 min/sample) and requires
no sample preparation.

Kearsley A T, Colaux J L, Ross D K, Wozniakiewicz P J, Gerlach L, Anz-Meador P, Griffin T, Reed B, Opiela J, Palitsin V V, Grime G W, Webb R P, Jeynes C, Spratt J, Salge T, Cole M J, Price M C, Burchell M J (2017) Hypervelocity impact in low earth orbit: finding subtle impactor signatures on the Hubble Space Telescope, Procedia Engineering 204 pp. 492-499 Elsevier
Return of materials from the Hubble Space Telescope (HST) during shuttle orbiter service missions has allowed inspection of large numbers of hypervelocity impact features from long exposure at about 615 km altitude in low Earth orbit (LEO) [1,2]. Here we describe the application of advanced X-ray microanalysis techniques on scanning electron microscopes (SEM), microprobes and a 2 MV Tandetron, to nearly 400 impacts on the painted metal surface of the Wide Field and Planetary Camera 2 (WFPC2) radiator shield [3,4]. We identified artificial Orbital Debris (OD) and natural Micrometeoroid (MM) origins for small [5] and even for larger particles [6], which usually may leave little or no detectable trace on HST solar arrays, as they penetrate through the full cell thickness [2,7].
Costa Catia, van Es Elsje M., Sears Patrick, Bunch Josephine, Palitsin Vladimir, Mosegaard Kirst, Bailey Melanie (2019) Exploring Rapid, Sensitive and Reliable Detection of Trace Explosives Using Paper Spray Mass Spectrometry (PS?MS), Propellants, Explosives, Pyrotechnics 44 (8) pp. 1021-1027 Wiley-VCH Verlag GmbH & Co
In this publication we work towards providing fast, sensitive and selective analysis of explosive compounds collected on swabs using paper spray mass spectrometry. We have (a) increased the size of the paper spray substrate to 1.6×2.1 cm for compatibility with current practise
in swabbing for explosive material; (b) developed a method for determining a successful extraction of analyte from the substrate to reduce false negative events; and (c) expanded the range of analytes that can be detected using paper spray to include the peroxide explosive HMTD, as well as nitroglycerine (NG), picric acid (PA) and tetryl. We report the development of a 30 s method for the simultaneous
detection of 7 different explosive materials using PSMS with detection limits below 25 pg, as well as detection of HMTD at 2500 pg, showing an improvement on previously published work.
Costa Catia, Frampas Cecile, Longman Katherine A., Palitsin Vladimir, Ismail Mahado, Sears Patrick, Nilforooshan Ramin, Bailey Melanie J. (2019) Paper spray screening and LC-MS confirmation for medication adherence testing: a two-step process, Rapid Communications in Mass Spectrometry Wiley

RATIONALE: Paper spray offers a rapid screening test without the need for sample preparation. The incomplete extraction of paper spray allows for further testing using more robust, selective and sensitive techniques such as liquid chromatography mass spectrometry (LC-MS). Here we develop a two-step process of paper spray followed by LC-MS to (1) rapidly screen a large number of samples and (2) confirm any disputed results. This demonstrates the applicability for testing medication adherence from a fingerprint.

METHODS: Following paper spray analysis, drugs of abuse samples were analysed using LC-MS. All analyses were completed using a Q Exactive" Plus Orbitrap" mass spectrometer. This two-step procedure was applied to fingerprints collected from patients on a maintained dose of the antipsychotic drug quetiapine.

RESULTS: The extraction efficiency of paper spray for two drugs of abuse and metabolites was found to be between 15-35% (analyte dependent). For short acquisition times, the extraction efficiency was found to vary between replicates by less than 30%, enabling subsequent analysis by LC-MS. This two-step process was then applied to fingerprints collected from two patients taking the antipsychotic drug quetiapine, which demonstrates how a negative screening result from paper spray can be resolved using LC-MS.

CONCLUSIONS: We have shown for the first time the sequential analysis of the same sample using paper spray and LC-MS, as well as the detection of an antipsychotic drug from a fingerprint. We propose that this workflow may also be applied to any type of sample compatible with paper spray, and will be especially convenient where only one sample is available for analysis.

Grime G.W., Sani S.F. Abdul, Palitsin Vladimir, Shafiqah A.S. Siti, Maah M.J., Alyahyawi Amjad, Bradley D.A. (2019) Simultaneous microbeam IBA and beam-induced luminescence analysis of strained doped silica fibre radiation dosimeters, Radiation Physics and Chemistry 155 pp. 173-177 Elsevier
We demonstrate that the simultaneous combination of ion beam analysis (IBA) and ion beam induced luminescence (IL) can reveal valuable information concerning the performance of strained doped silica fibre thermoluminescence microdosimeters. The micron scale spatial resolution and low detection limits of IBA allow the lateral distribution of dopant elements to be mapped and then correlated with the distribution of prompt radioluminescence. Measurement of the decay of the IL signal with dose provide information concerning the saturation of the subsequent TL signal at high doses. MeV ion beams can deposit relatively high energy in localized, well-quantified small volumes and so this method is valuable for studying high dose effects in TL dosimeters. We describe a simple modification of the target chamber microscope which enables sensitive low background light detection in two wavelength bands and present preliminary results from three types of germanium doped silica fibre dosimeter.
Matja
i? L., Palitsin V., Grime G.W., Abdul-Karim N., Webb R.P.
(2019) Simultaneous molecular and elemental mapping under ambient conditions by coupling AP MeV SIMS and HIPIXE, Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 450 pp. 353-356 Elsevier
Ion Beam Analysis (IBA) consists of a set of analytical techniques addressing elemental composition of inorganic material normally conducted using ion beams in the MeV kinetic energy range. Secondary Ion Mass Spectrometry using MeV ions (MeV SIMS) is the only IBA technique which can provide extensive molecular information about organic materials. MeV ions can be extracted into air hence offering the potential to apply MeV SIMS under atmospheric pressure. At the University of Surrey Ion Beam Centre, a fully ambient MeV SIMS setup has been developed and termed ?Ambient Pressure MeV SIMS?. This AP MeV SIMS can be optimized for analysis and imaging of organic molecules. MeV SIMS relies upon electronic sputtering of the target material and this is much more efficient in insulating or organic targets, and less efficient in conducting metallic materials. PIXE, on the other hand, is efficient at providing good signals from elemental metallic systems, but does not readily provide molecular information from organics. The combination of the two techniques ? preferably simultaneously with the same beam ? provides useful complementary information which can readily be combined. Here we present pioneering preliminary work in simultaneous molecular and elemental imaging of a complex sample comprising of two organic species and two metallic species by combining AP MeV SIMS with Heavy Ion Particle Induced X-ray emission (HIPIXE).
Matjacic Lidija, Palitsin Vladimir, Demarche Julien, Rosa Lucio, Stori Elis M., Webb Roger (2019) Optimisation of secondary ion transport in ambient pressure MeV SIMS, Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 448 pp. 1-4 Elsevier
Ambient Pressure MeV SIMS (AP MeV SIMS) is a special application of MeV SIMS technique for molecular detection and imaging under ambient conditions. There are several advantages of using ambient over nonambient techniques such as minimising or completely avoiding sample preparation that can contribute to the reducing of costs and shortening of analysis. Moreover, by performing analysis in ambient conditions negative vacuum influence on samples will be avoided. The emergence of ambient mass spectrometry techniques over the
past decade has been enormous with a broad range of applications such as food quality, environmental analysis and life sciences [1,2]. On the other hand, the disadvantage of ambient pressure mass spectrometry techniques is the influence of the ambient background which can suppress the signal from the target. In AP MeV SIMS, molecular species present in ambient surrounding of the sampling site will also be ionised by ion beams hence secondary ions originating from the sample have to be transported in the most efficient manner from the site of
interaction of ion beams and target into the mass spectrometer capillary and, finally, into the mass spectrometer [3]. In this work, we present the optimisation of the mass spectrometer capillary temperature, distances of mass spectrometer and sheath gas, in our case helium, with respect to the beam axis and angle of the helium flow capillary with respect to the sample.
Grime G.W., Al-Shehri S., Palitsin V. (2019) A simple edge-following scanning algorithm for proton beam writing and other direct-write lithographies, Journal of Micromechanics and Microengineering 29 (3)

The quality of the structures fabricated using proton beam writing (PBW) and other direct-write microfabrication methods is strongly influenced by the path followed by the writing beam during the exposure. In particular, it is necessary to avoid paths in which the beam makes large jumps or changes in direction close to the edges of the structure, and ideally the scan path should follow the outline of the pattern to be exposed (sometimes referred to as turtle scanning). While this is relatively easy to implement when the patterns to be created can be built up from simple geometric shapes (circles, rectangles, etc), it has not been possible to do this in the case of arbitrarily complex images, at least using software available to the PBW community.

This paper describes a simple edge-following algorithm (EFA) which uses a method of spiral searching around each pixel to determine a scan path which not only optimizes the conformity of the scan path to the edges of the required pattern, but also minimizes jumps (and hence blanking time) and scan reversals which can cause artefacts due to scanning system transients. The EFA operates on a 1-bit BMP format input image file and has been implemented in the OMDAQ-3 software package (Oxford Microbeams Ltd).

The paper is illustrated with examples of complex structures written using the EFA at the University of Surrey Ion Beam Centre which demonstrate enhanced edge smoothness compared with simple blanked raster scanning.

Costa Catia, van Es E.M., Sears P., Bunch J., Palitsin Vladimir, Cooper H., Bailey M.J. (2019) Exploring a route to a selective and sensitive portable system for explosive detection? swab spray ionisation coupled to of high-field assisted waveform ion mobility spectrometry (FAIMS), Forensic Science International: Synergy 1 pp. 214-220 Elsevier
Paper spray mass spectrometry is a rapid and sensitive tool for explosives detection but has so far only been demonstrated using high resolution mass spectrometry, which bears too high a cost for many practical applications. Here we explore the potential for paper spray to be implemented in field applications with portable mass spectrometry. This involved (a) replacing the paper substrate with a swabbing material (which we call ?swab spray?) for compatibility with standard collection materials; (b) collection of explosives from surfaces; (c) an exploration of interferences within a/±/0.5/m/z window; and (d) demonstration of the use of high-field assisted waveform ion mobility spectrometer (FAIMS) for enhanced selectivity. We show that paper and Nomex® are viable collection materials, with Nomex providing cleaner spectra and therefore greater potential for integration with portable mass spectrometers. We show that sensitive detection using swab spray will require a mass spectrometer with a mass resolving power of 4000 or more. We show that by coupling the swab spray ionisation source with FAIMS, it is possible to reduce background interferences, thereby facilitating the use of a low resolving power (e.g. quadrupole) mass spectrometer.
Lewis Holly-May, Webb Roger, Verbeck Guido F, Bunch Josephine, De Jesus Janella, Costa Catia, Palitsin Vladimir, Swales John G., Goodwin Richard J. A., Sears Patrick, Bailey Melanie Jane (2019) Nanoextraction coupled to liquid chromatography mass spectrometry delivers improved spatially resolved analysis, Analytical Chemistry American Chemical Society
Direct analyte probed nanoextraction (DAPNe) is a technique that allows extraction of drug and endogenous compounds from a discrete location on a tissue sample using a nano capillary filled with solvent. Samples can be extracted from a spot diameters as low as 6 µm. Studies previously undertaken by our group have shown that the technique can provide good precision (5%) for analysing drug molecules in 150 µm diameter areas of homogenised tissue, provided an internal standard is sprayed on to the tissue prior to analysis. However, without an isotopically labelled standard, the repeatability is poor, even after normalisation to and the spot area or matrix compounds. By application to tissue homogenates spiked with drug compounds, we can demonstrate that it is possible to significantly improve the repeatability of the technique by incorporating a liquid chromatography separation step. Liquid chromatography is a technique for separating compounds prior to mass spectrometry (LC-MS) which enables separation of isomeric compounds that cannot be discriminated using mass spectrometry alone, as well as reducing matrix interferences. Conventionally, LC-MS is carried out on bulk or homogenised samples, which means analysis is essentially an average of the sample and does not take into account discrete areas. This work opens a new opportunity for spatially resolved liquid chromatography mass spectrometry with precision better than 20%.
Jeynes Christopher, Palitsin Vladimir, Kokkoris M., Hamilton A., Grime Geoffrey (2020) On the accuracy of Total-IBA, Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 465 pp. 85-100 Elsevier
?Total-IBA? implies the synergistic use of multiple IBA techniques. It has been claimed that Total?IBA inherits the accuracy of the most accurate IBA technique used. A specific example is now given of this where (in vacuo) EBS/PIXE of a glass sample uniform in depth is validated against absolutely calibrated EPMA of the same sample. The EPMA results had a mass closure gap of 2.0 ± 0.6 wt%; the full PIXE analysis determined the composition of this missing 2 wt%. The PIXE calibration was against a single certified glass sample, with uncertainties per line ~10%. Benchmarking also demonstrates ~10% underestimation of the Si scattering cross-section at proton energies ~3 MeV. But the Total-IBA determination of the silica content had a low standard uncertainty of about 2%. This is due to the strong constraints of both the chemical prior and also the mass closure properties of the EBS. Irradiation-induced sodium migration in this soda-lime glass is explored.
This thesis describes the use of proton beam writing (PBW) for the fabrica- tion for microfluidic and microelectromechanical system (MEMS) devices. In particular, the fabrication of three-dimensional (3D) micro or nanostruc- tures with high aspect ratios is of growing interest in these fields. PBW is the only technique that has the capability to satisfy these requirements while providing full control of the geometrical parameters, such as the sur- face roughness and side wall angle. This technique is a direct microfabri- cation method that employs a focused, energetic (MeV) proton beam to structure the input pattern in resist materials.
In the present work, a network of buried channels is fabricated as part of a project to develop a functional microfluidic device for neuronal studies and self-powered microfluidics (capillary micropump). Proton beam with energies of 0.75 to 2.5 MeV is used to fabricate the channels in 3D with a minimum feature size of approximately 1 ¼m and depths of 40 to 60 ¼m. The roughness of the sidewalls of the written channels is approximately 3 nm root mean square roughness (Rrms).
Radio frequency (RF) MEMS switches, which consist of an overhanging structure, are also written using PBW, and new MEMS switch designs are proposed. These designs are constructed so as to provide full control of the main cantilever beam parameters, such as the thickness, spring constant, and actuation.
The three main stages of the lithography process, i.e., pre-exposure, expo- sure, and post-exposure, are investigated and optimised for application to poly(methyl methacrylate)(PMMA), pure SU-8 polymer, and SU-8/silver- nanoparticle nanocomposites (SU-8/AgNp). During the exposure process, the proton beam energies, doses, and scanning method are also optimised, in order to attain a good-quality structure (i.e., a robust structure with smooth and straight walls). The mechanical and electrical properties of the nanocomposites, which are irradiated with a range of proton beam doses, are measured.
Note that the structures written in this work are numerically validated prior to the writing process using COMSOL Multiphysics ýR software. The fluid flow in the written buried channels is investigated using numerical methods.
Jang Min, Costa C., Bunch J., Gibson B., Ismail M., Palitsin Vladimir, Webb Rebecca, Hudson M., Bailey M.J (2020) On the relevance of cocaine detection in a fingerprint, Scientific Reports 10 1974 Nature Research
The finding that drugs and metabolites can be detected from fingerprints is of potential relevance to forensic science and as well as toxicology and clinical testing. However, discriminating between dermal contact and ingestion of drugs has never been verified experimentally. The inability to interpret the result of finding a drug or metabolite in a fingerprint has prevented widespread adoption of fingerprints in drug testing and limits the probative value of detecting drugs in fingermarks. A commonly held belief is that the detection of metabolites of drugs of abuse in fingerprints can be used to confirm a drug has been ingested. However, we show here that cocaine and its primary metabolite, benzoylecgonine, can be detected in fingerprints of non-drug users after contact with cocaine. Additionally, cocaine was found to persist above environmental levels for up to 48 hours after contact. Therefore the detection of cocaine and benzoylecgonine (BZE) in fingermarks can be forensically significant, but do not demonstrate that a person has ingested the substance. In contrast, the data here shows that a drug test from a fingerprint (where hands can be washed prior to donating a sample) CAN distinguish between contact and ingestion of cocaine. If hands were washed prior to giving a fingerprint, BZE was detected only after the administration of cocaine. Therefore BZE can be used to distinguish cocaine contact from cocaine ingestion, provided donors wash their hands prior to sampling. A test based on the detection of BZE in at least one of two donated fingerprint samples has accuracy 95%, sensitivity 90% and specificity of 100% (n = 86).