Irish Isotopes Research Group

Analytical Equipment across Member sites

December 2013, v.1.0

14CHRONO, BelfastDirector: Prof. Paula ReimerEmail: p.j.reimer@qub.ac.uk

Facility Webpage: http://www.chrono.qub.ac.uk/

The 14CHRONO Centre operates a NEC compact 0.5 MV accelerator mass spectrometer. Sample pretreatment, graphitisation and analysis is car-ried out by an experienced team. Our facility can analyze submilligram samples of carbon – either organic (bone collagen, cremated bone, hair and other tissues, wood, plant macrofossils, sediment, dissolved organic carbon etc.) or inor-ganic (shell, coral, speleothem groundwater etc.)

Thermo Delta V IRMS with Flash EA

The IRMS is used exclusively for δ13C and δ15N on organic matter. We analyse a range of sample types – collagen, cellu-lose, plant material, hair and animal tissues.

NEC compact 0.5 MV AMS

QUB Stable Isotope Facility

Labratory Manager: Dr Neil OgleEmail: n.ogle@qub.ac.uk

Twitter: @neilogleFacebook: Stable Isotope Facility QUB

Thermo Delta V IRMS with Thermo

TC/EA and Thermo Flash 1112

Our Thermo TC/EA has a dual role in being able to

measure both δ18O and δ2H of waters and solids.

Our Flash 1112 is dedicated to δ34S analysis and as with oxygen and hydrogen a varied mix of projects and sample type has been measured with this set-up.

Analytical Precision 2003 IRMS

This IRMS is dedicated to the measurement of δ13C and δ18O from carbonates. The machine has also previously contributed to the medical profession by being able to isotopically meas-ure breath gas for gastro-intestinal dysfunction.

Isoprime IRMS with Eurovector EA

This IRMS is used exclusively for δ13C and δ15N on organic matter. A range of sample mate-rial has been passed through the system – cellu-lose, foodstuffs, soil etc and a number of projects have used the system, presently though it has been principally for the food science community.

The Stable Isotope Facility has a further two IRMSs with a range of peripherals that are currently in hi-atus as they await suitable projects to utilise them and the lab manager is always willing to discuss and collaborate on any potential initiative. Note though that a small investment of a few thousand pounds in each case would be required to bring the systems back to accepted operational performance.

The first is our second ISOPRIME which has been recently refurbished but has been un-derused since. When it was in use it was for nitrate (δ15N) analysis in waters utilis-ing a labmade preparation and delivery unit.

The second IRMS is a Thermo Delta Plus Ad-vantage. It has two peripheral devices at-tached, one with a GC assembly for δ13C analy-sis of specific compounds from a liquid injection and the second a Thermo ISOLINK which has been used for the δ13C analysis of DIC in waters.

IT Sligo, Environmental

Science IIRG Member: Carmel Moran

Email: moran.carmel@itsligo.iewww.facebook.com/EnvironmentalScienceITS-

ligo

Varian 710: Inductively Coupled Plasma Atomic Emission (ICPAES)

spectrometer system

•Large dynamic range for determination of major, minor and trace elements in a single analytical

run.•Solid state RF generator and plasma generation

system.•Standard solution sample introduction system with flexible interchange of various nebulisers.

•Flexible interfacing of alternative sample intro-duction including hydride generation and high

efficiency nebulisers.•Wavelength coverage: 170- 900 nm (approx)

•Charge coupled device based detector (recircu-lating cooler)

•Resolution:0.01-0.001nm•Rapid and flexible selection of spectral lines

•Rapid Automated acquisition of multi-element data

•Background correction capabilities•User friendly software

•Argon plasma gas •Compact bench-top dimensions

Inductively Coupled Plasma Mass Spectrometer (ICPMS)

•Quadrupole based low resolution ICPMS instru-ment (Varian 820 ICPMS)•Large dynamic range for determination of major, minor and trace elements in a single analytical run.•Low resolution isotopic analysis capability for analysis of heavy metals (resolution 0.5 amu). Not suitable for carbon, nitrogen or oxygen isotopic analysis due to solution based sample introduc-tion system. •Solid state RF generator and plasma generation system.•Automated plasma generation and control for various operational modes including ‘cool plasma’ mode•Compact design and vacuum system•Rapid pump down and optimisation•Automated instrument setup and analytical opti-misation system•Collision/reaction cell (easy changeover for use both with and without reaction cell) utilising hy-drogen, helium, etc.•Cooling system for spray chamber, coils, etc.•Low spectral background and interference.•Flexible operation in qualitative(spectral display), semi-quantitative and quantitative analysis•Standard solution sample introduction system with flexible interchange of various nebulisers.

Wavelength Dispersive XRF Also available - please contact site for details.

TCD Geology Department

IIRG Member: Dr Quentin CrowleyEmail:

Website:http://www.tcd.ie/Geology/geochemfa-cility/

Clean laboratory for ultra-low blank preparation of samples.

Quadrupole ICP-MSboth laser ablation and solution mode capabilities. Used for trace ele-ment and isotope ratio measurements.

ICP-OES this has not arrived yet, but will be cou-pled to the quad ICP-MS, so that we can do simultaneous major elements.

CF-IR-MS for C-N mainly on carbonates and phosphates and O for waters.

XRD (X-Ray) diffraction - used for iden-tification of fine grained minerals.

SEM imaging (with the Centre for Micros-copy and Analysis at TCD).

NCIG, UCD Geological

Sciences (UCD, TCD, UCC)

IIRG member: Prof. Stephen DalyEmail:

Website: http://www.ucd.ie/geology/ncig.html

Thermoscientific Triton multiple collector thermal ionisation MS

High precision isotope ratio and isotope dilution measurements in the Rb-Sr, Sm-Nd and U-Th-Pb isotopic systems.Capable of many more techniques (e.g.Ca, and in negative ion mode for Re-Os)

Thermoscientific Neptune multi-ple collector ICP -MS

Equipped with ion counters as well as Faraday detectors. High precision isotope ratio analyses of Sr, Nd, Pb, Fe, Cu, Zn,Lu-Hf, U-Th in solution mode.

Of particular potential interest to the Archaeologi-cal community is its capability for U-Th dating of bone, tooth enamel and speleothem calcite, as well as heavy stable isotopes (Pb, Zn, Fe, Cu) of metal artefacts and Sr+Pb in various materials.

Measurement in ion counting mode allows in situ analysis (using the laser, no. 3 below) of very small sample volumes, or of solu-tions with very low elemental concentrations.

New Wave Excimer (193nm) laser ablation system

This is coupled with the Neptune and is mainly used for in situ analysis of Pb (es-pecially in Kfeldspar) and Lu-Hf in zircon. It is also capable of high precision U-Pb anal-ysis of the U-Pb system in various minerals.

New Wave Micromill

For microscale (10 micron spots or rasters) sampling of a variety of materials - current-ly used mainly for speleothems and feldspars but readily applicable to bone and tooth mate-rial. Samples prepared using the Micromill are digested chemically and analysed in solution.

Solution analyses are generallymore reliable than laser-ablation analyses be-cause they are subject to less complicated (more predicatble and more reproducible) matrix ef-fects. Hence, selected regions of material ana-lysed using the laser can be sampled in near-replicate using the Micromill in order to validate laser-ablation analytical data from the same sample.

Desktop Scanning Electron Microscopy

With Back-scattered electron (BSE) imag-ing and Energy-dispersive X-ray (ie chemi-cal compositional) analyses down to c. 4 mi-cron spatial (and c. 6 micron depth) resolution.

1. We are in the process of acquiring a Quad-ropole inductively coupled plasma mass spec-trometer, which will be capable of analysing a wide range of minor and trace elements either in solution or in situ coupled with the laser.

By coupling the laser ablation sampling system to the Quadropole and Neptune simultaneously, it will be possible to carry out simultaneous trace element analyses with the Quadropole while measuring selected isotope ratios on the Neptune.

2. Clean-air low-blank chemical facilities for sam-ple digestion and ion exchange chromatography

3. General sample preparation facilities in-cluding rock crushing, mineral separation using standard magnetic and density/ flotations meth-ods, high precision thin section and polishing.

We are very well equipped with a wide range of reference materials for compositional and iso-tope ratio analysis and have a good archive par-ticularly of Sr, Nd and Pb isotope ratio measure-ments on “standard reference” materials. These data are available (as appropriate) in publications using data from the NCIG labs. Details on request and available (eventually) on the NCIG website.

NCIG, continued