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The self-consistent Ion Beam Analysis (IBA) of cultural heritage samples using the external beam is technically demanding. We report on the calibration of an analysis of glass samples from the Rosslyn Chapel where the interest will ultimately be in the full characterisation of the weathered glass. Such an analysis requires a comprehensive Total-IBA approach using p-PIGE and He-PIXE to obtain ”bulk” and surface Na, with H-PIXE/EBS for multielemental depth profiling to 10 μm and He-PIXE/EBS for higher depth resolution near the surface; also with two PIXE detectors as usual for the high and low energy parts of the spectrum. A revised NDF v.10 code capable of a self-consistent handling of all these signals at state-of-the-art accuracy is described, together with the calibration protocols required for such an analysis. Other capabilities of the NDF code not previously discussed are also reviewed.

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).

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.

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.

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.

“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.

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. Keywords: Explosives, Swab spray, Mass spectrometry, FAIMS

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.

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 μm and depths of 40–55 μm. 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.

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.

Sample elemental concentrations can be determined using the microbeam proton-induced X-ray emission (PIXE) technique, providing non-destructive simultaneous low-background multi-element analysis. Present interest concerns analysis of Ge-doped SiO2 fibres intended as high spatial-resolution thermoluminescence (TL) dosimeters for radiation measurements in place of their more typical applications in telecommunications. During fibres fabrication, defined amounts of the Ge dopant are added, the dopant more usually having a determining role in the transmission properties of the fibre. Characteristic X-rays produced in PIXE analysis provide information on the relative distribution of elements within a sample, as in for instance Ge and Si concentrations, the Ge acting as point defect centres that promote TL. With the dopant tending to diffuse in and away from the fibre core, it is essential to define the sample matrix composition in order to accurately evaluate the X-ray yield. This is determined in part using simultaneous Rutherford Back Scattering analysis. In present work, PIXE/Rutherford Back Scattering measurements have been employed to ascertain dopant concentrations of fibres that have been fabricated at the University of Malaya with a view to improving TL yield. Present results concern cylindrical fibres, nominally with 4%, 6% and 8% weight peak Ge concentrations and flat fibres of nominal 6% weight Ge concentration. For the cylindrical fibres, Ge dopant concentration has been found to be in the range of 2.41–4.56%, 6.44–8.29% and 10.27–12.25% weight, respectively, while for the flat fibres, the Ge concentration range is broader, at 0.07–6.55% weight. Copyright © 2014 John Wiley & Sons, Ltd.

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.

The primary beam energy and species (Cs + , Ar + ) dependence of ultra low energy SIMS depth profiles of ultra-shallow boron implants into CVD grown diamond is investigated in this paper. The data are compared with TRIM simulation of the 5 keV 11 B + implant. Cs + profiles (1 keV, 30°) appear to be seriously distorted by atomic mixing and recoil implantation due to the high mass of the probe. Ar + profiles (300 eV-1 keV, 0°) are less distorted, but both Cs + and Ar + tend to produce significant tails. The Ar + SIMS profiles produce implants which appear to be shallower than the TRIM simulation. We show that profiling using Ar + with energies between 0.3 and 1 keV can be used to extrapolate a profile to zero beam energy. The extrapolated data indicate a centroid between 5 and 10 nm from the surface, whereas TRIM predicts 11 nm.

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.

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.