SERVICES & FACILITIES ANNUAL REPORT - FY April 2006 to March 2007 SERVICE Life Sciences Mass Spectrometry Facility (LSMSF) FUNDING Block AGREEMENT EK: R8/H10/09 L: R8/H10/20 B: -R8/12/15 ESTABLISHED as S&F East Kilbride Lancaster Bristol TERM 5 years 1994 1984 1992 TYPE OF SERVICE PROVIDED: Facility: Under the auspices of the LSMSF, NERC maintains three facility nodes for provision of organic and light stable isotope mass spectrometry to the UK life sciences community, namely the East Kilbride node located at SUERC, the Lancaster node located within CEH-Lancaster and the Bristol node housed within the School of Chemistry at the University of Bristol. By adopting this more integrated approach accessibility to said Facility nodes has been increased as has been the organisation between Facilities. Whilst this move has not resulted in the physical amalgamation of the three Facilities, the ‘one-stop-shop’ exists as a single point of contact for users, with increased efficiency and synergistic operation thus making better use of the resources currently used in the maintenance of the mass spectrometry services offered. All three Facilities are contracted by NERC to provide ‘free-at-point-of-delivery’ support according to their respective service level agreements (SLAs) or contracts and the NERC LSMSF steering committee oversees their operation. Each of the three nodes offers a different portfolio of analytical techniques for which UK based researchers may apply to use through NERC Services and Facilities (S&F) by standard peer review procedure. East Kilbride has strong associations with migration, agro-ecology and conservation studies whilst the primary remit of Lancaster is terrestrial and fresh-water studies (including those deriving from NERC programmes). Bristol fields a wide range of projects to which a compound specific approach is essential, e.g. palaeoclimatic reconstruction (alkenone UK37), organic matter sourcing (biomarkers), faunal population and dietary studies (isotopic PLFA and FFA profiling) and palaeodietary reconstruction. Analytical portfolio of the LSMSF: Isotopically enriched water (D218O to energy expenditure studies Natural abundance e.g. 13C/12C, 15N/14N, 18O/16O and 34S/32S analyses of bulk animal organic matter & molecular oxygen to study food webs & element cycling Enriched & natural abundance analyses of bulk terrestrial organic matter e.g. 13C/12C, 15N/14N Enriched & natural abundance analyses of gases: e.g. 13C/12C, 15N/14N 18O/16O of CO2, CH4, N2O & N2 Natural & near natural abundance compound specific 13C/12C, 15N/14N, D/H analyses of biochemical extracts Organic mass spectrometric analyses of complex mixtures of compounds e.g. volatiles, functionalised molecules etc NB. Nodes are designated as follows: L = Lancaster, EK= East Kilbride, B = Bristol ANNUAL TARGETS AND PROGRESS TOWARDS THEM Lancaster node to: a) continue to provide existing accredited methodologies for customers, b) to develop existing technology to achieve accurate/precise measurements on smaller quantities of materials c) to continue with staff and student training under the remit of the LSMSF. Progress has been successful for all three targets. EK Node to: develop dual hydrogen-oxygen analysis in organic materials to the point that it is a routine analysis. Bristol node to: to develop compound specific D and 15N analytical methodologies towards the goal of making them routine Facility services. This has been successful although both techniques will remain more time consuming than other analyses. SCORES AT LAST REVIEW (each out of 5) Need Uniqueness 5 5 CAPACITY of HOST ENTITY FUNDED by S&F Lancaster East Kilbride Bristol 58% 100% 13% Quality of Service 5 Date of Last Review: Quality of Science & Training 5 Staff & Status Dr AW Stott (SSO), Mr D. Sleep (HSO), Miss H. Grant (SO) Dr. J Newton (RA2) & Dr. R. McGill (RA1A) Dr. ID Bull (OR2; 100% University of Bristol funded) & Dr. R Berstan (RA1A) FINANCIAL DETAILS: CURRENT FY Total resource Unit Cost £k allocation £k ½ day unit Analysis Training/Labwork EK 141.69 EK 406 L 95.66 L 386 B 71.42 B 846 FINANCIAL COMMITMENT (by year until end of current agreement) 2007-08 EK 159.08 2008-09 EK c164 L 92.27 L 95.13 B 123.84 B c.127.67 STEERING COMMITTEE LSMSF Independent Members 5 Meetings per annum 2 28/01/03 Average 5 Next Review (January) 2008 Capital Expend £k 0 0 12.57 Other S&F Overseen 0 Income £k 0 0 0 Contract Ends (31 March) 2009 Full cash cost £k 172.93 117.23 93.95 APPLICATIONS: DISTRIBUTION OF GRADES (Current FY — 2006/07) R*/Pilot 5 4 3 2 1 NERC Grant projects 1 1 0 0 0 0 1 Other academic 4 4 0 1 0 0 1 Students 3 8 7 0 0 0 2 Pilot 0 0 0 0 0 0 0 8 13 7 1 0 0 4 TOTAL APPLICATIONS: DISTRIBUTION OF GRADES (per annum average previous 3 years —2003/04 –2005/06 R*/Pilot 5 4 3 2 1 NERC Grant projects 0 6 0.33 0 0 0 1 Other Academic 0 3.66 1 0 0.33 0 1.33 Students 0.33 3.66 3.33 0 0 0 2.66 Pilot 0 0 0.33 0 0 0 0 0.33 13.33 5.0 0 0.33 0 5.0 TOTAL PROJECTS COMPLETED (Current FY) 5 NERC Grant projects 2 Other Academic Students Pilot 4 2 3 7 3 1 2 Infrastructure Grand Student Supplement to NERC NERC Total Other Grant * RC Total NERC 89 7 55 24 7 20 USER PROFILE (per annum average previous 3 years- 2003/4-2005/06 Infrastructure Grand Student Supplement to NERC NERC Total Other Grant * RC Total NERC 58.66 11.33 32 19 6.33 12.33 NERC Grant* 0 NERC Grant* 0 OUTPUT & PERFORMANCE MEASURES (current FY) Publications (by science area & type) SBA ES MS AS TFS EO Polar Grand Total Refereed 15 0 73.2% 0 *Combined non-Directed and Directed PAYG Student NERC Other C/S Total NERC 0 0 0 0 *Combined non-Directed and Directed PAYG Student NERC Other C/S Total NERC 0 0 0 0 PhD 55 Commercial 2 PhD 29.33 Commercial 1.66 Non-Ref/ Conf Proc 19 0 67 42 Distribution of Projects (by science areas) SBA ES MS AS TFS EO 8.8% 0.9% 38.0% 5.9% 42.6% 2.9% OUTPUT & PERFORMANCE MEASURES (per annum average previous 3 years 2003/4-2005/06) Publications (by science area & type) SBA ES MS AS TFS EO Polar Grand Total Refereed Non-Ref/ Conf Proc 5.33 2.66 7.33 0 32.66 0 0 48 32.66 8.66 Distribution of Projects (by science areas) SBA ES MS AS TFS EO 6.5% 1.6% 22.0% 0.0% 69.9% 0.0% Earth’s Life Support Systems 36 R*/Pilot 2 USER PROFILE (current FY) Academic NERC RC NERC Fellows 29 4 1 USER PROFILE (per annum average previous 3 years 2003/4-2005/06) Academic NERC RC NERC Fellows 21.66 6.33 1.66 14 Reject 0 0 0 0 0 3 USER PROFILE (current FY) 2 1 Reject 0 0 1 0 1 Distribution of Projects (by NERC strategic priority) Climate Change Sustainable Economies Underpinning Science 7.1% 15.9% 3.8% PhD Theses 6 Polar 0.9% PhD Theses 6.66 Polar 0.0% Specific Research 0.0% OVERVIEW & ACTIVITIES IN FINANCIAL YEAR (2005/06):Node overview East Kilbride: This has been a busy year with a record number of successful applications to the node, most of which required 13C and 15N analysis. We are receiving much interest in dual 2H and 18O analysis to track the migratory behaviour of birds and insects, including two applications from the October round; thus we are in the process of formalising this technique such that it becomes a routine procedure in our portfolio. Peer-reviewed publications from node staff numbered seven, with a similar number already accepted for 2007-08. We were heavily involved with the organisation of the 5th International Conference on Applications of Stable Isotope Techniques to Ecological Studies in Belfast, with a view to publicising the work of the LSMSF to an international audience, and as a result have received several enquiries from UK-based researchers. Lancaster: 2006/2007 has seen a busy year with a steady influx of samples into the laboratory from the NERC approved applications covering the full suite of techniques offered within the remit of the node. The EA-IRMS 13C and 15N and trace gas CO2 methods have again been internally and externally audited as part of UKAS ISO 17025 and have been found fit for purpose and operating to the highest standards. The number of external enquiries received this year was 12, resulting in eight applications to the LSMSFSC, one of which was referred to the NIGFSC. Publications from node staff amounted to seven this year. Visiting PhD students trained in stable isotope methodologies, specifically trace gas CO2 and bulk 15N summed to a total of six. The node staff participated in 5th International Conference on Applications of Stable Isotope Techniques to Ecological Studies in Belfast (organised by LSMSF East Kilbride/Queens University), August 2006 with the aim to promote the LSMSF to a wider audience. Bristol: The 2006/2007 period has been somewhat challenging due predominantly to factors beyond the control of the Facility node. Large scale refurbishment of the building housing the Facility has inevitably resulted in a number of disruptions arising primarily from downtime of air conditioning units, flooding incidents and general building work. Despite these hindrances the node was operational for most of the year and has so far fulfilled 63% of its NERC allocation for this period. Inability to fulfil the remaining commitment arises from the loss of personnel at institutions currently in receipt of successful applications to NERC LSMSF resulting in a lack of provision of samples for analysis within scheduled timeframes. The losses of personnel are regrettable but the Bristol node will endeavour to analyse outstanding samples whilst fulfilling into contractual obligations to NERC over the ensuing 2007/2008 period. Work supported by the node has resulted in another 2 peer-reviewed publications whilst Facility and associated staff have generated a further 20 publications (17 peer-reviewed papers and 3 PhD theses). Both Drs Bull and Berstan participated in 5th International Conference on Applications of Stable Isotope Techniques to Ecological Studies in Belfast (organised by LSMSF East Kilbride/Queens University), August 2006 with the aim to promote the LSMSF to a wider audience. Generic LSMSF training protocol: One of the primary goals of the LSMSF strategy is to actively underpin Ph.D. student and postdoctoral training. During 2006, a record of 34 applications were received by the LSMSFSC for review, 62 % of these projects supporting PhD student research projects. Students have had little if any previous experience of ‘wet chemical’ preparative methodologies, high precision quantitative stable isotope analyses or mass spectrometry and this was their first introduction to vacuum-line cryogenic chemistry and/or isotope-ratio mass spectrometry or related mass spectrometric techniques. The often intensive training they receive within the LSMSF therefore develops skills different and complementary to those required in the field or later in their career development. The combination of laboratory analysis and data interpretation skills is considered an attractive attribute of our 'alumni' and fulfills NERC’s responsibilities to students and fellows as part of their skill development portfolio. LSMSF Capital East Kilbride: No capital allocation was requested for this period. The small turbo pump on our Delta XP-Plus failed after only 4 years of service, but this was replaced using funds from the recurrent budget. Lancaster: No capital allocation was requested for this period. The trace gas IRMS 250l turbo pump failed in early March after 10 years of service and needed to be replaced from the recurrent budget. Bristol: A total of £12,570 was requested and granted in order to perform two upgrades to instrumentation maintained by the Facility. The first upgrade was the reconfiguration of the TraceMS single quadrupole mass spectrometer ion source to make it capable of performing CI ionisation thereby enabling replication of a technique previously provided by the now decommissioned TSQ700 MS. This purchase also included provision of a completely separate CI ion source that can be quickly inserted into the mass spectrometer as required (£5405). The second upgrade involved replacement of an electronics board and new software for the TraceMS thereby enabling a CTC Pal Autosampler to be used with this instrument. The CTC Pal Autosampler is a high-end state-of-the-art autosampler, purchased using funds obtained from HEFCE and the University of Bristol (~£10k), it combines the capability for high and reliable sample throughput with a wide range of user definable custom injection cycles including the capability for the automatic addition of a calibration standard. The reliability and extra functionality resulting from this upgrade will greatly benefit the continued high sample turnover and will improve the accuracy of data generated by the TraceMS for future samples submitted to the Bristol node (£7165). SCIENCE HIGHLIGHTS (including four most impactful outputs): East Kilbride: Richard Inger, a NERC-funded student working on “Aspects of winter and spring staging ecology in a long distance migrant”at Glasgow University under the supervision of Graham Ruxton and Stuart Bearhop (Exeter) has been using the 13C and 15N to predict the depletion of seagrass by these herbivores and their consequent diet-shift to terrestrial biomass using the probability model Isosource. He completed his thesis this year and has subsequently published two papers, one which describes the model itself (Journal of Applied Ecology 43, 1022-1030), and a second which describes the timing of the diet shift (Journal of Animal Ecology 75, 1190-1200). Two further manuscripts utilising this data have also submitted to Oecologia and Animal Behaviour. Lancaster: A NERC funded research project lead by Essex University in collaboration with the LSMSF Lancaster node has shown that three U.K estuaries (Colne, Humber, Conwy) which ranged from extremely nutrified to oligotrophic, were shown to be major sources of nitrous oxide and that the process of denitrificaton and N 2O formation were from benthic process, and not from watercolumn processes. For the first time, the formation of N 2O from either nitrification or denitrification steps of NO 3- generation within the sediment was determined (Limnology & Oceanography 51 (1/2), 545-557). A collaborative GANE research project between the University of York, CEH Bangor and the Lancaster node resulted in a publication in Atmospheric Environment 4, 498-507. Using Calluna vulgaris as a bio-monitor, it was possible to assess the zone of N deposition from high ammonia emission sources within just one year. Bristol: A supported collaboration between the University of Bristol and the Environmental Change Research Centre, University College London focussed on qualitative and quantitative analysis of a range of higher plant and algal biomarkers in Amazon Fan sediments (ODP Site 942). From from the results, changes in the vegetation and discharge history of the Amazon were inferred, with key observations being a massive input of sediments at about 10 Ka but a lack of any major change in Amazon Basin vegetation in the entirety of the record. The latter observation is highly significant as it is inconsistent with the Amazon Refugia model for high Amazonian rainforest diversity (Organic Geochemistry 37(2), 208-219). FUTURE DEVELOPMENTS/STRATEGIC FORWARD LOOK East Kilbride: Based on current applications and informal enquiries, we predict that dual 2H/18O analysis will become an important technique in our portfolio. We will shortly be undertaking some enriched 13C analyses using CF-IRMS. This diversification of analytical techniques and the concomitant increase in applications has motivated capital funding for 2007-2008 for a new mass spectrometer. Lancaster: Possible future growth areas are measurement of 15N of NH4+ & NO3- in ground waters and bulk 18O analyses on leaf material to measure water efficiency/droughting processes. A high temperature EA fitted with solid/liquid injection be required to carry out 18O analyses on plant material which will require capital input. It is foreseeable this will be a growth area in the near future and expansion of the nodes capability into this area will be certainly strategic in terms of the LSMSF’s techniques portfolio. Bristol: Over the next year the node will concentrate on the development of two new methodologies that it is anticipated will of be great benefit to the UK life sciences community. The first of these will be the adoption and development of a protocol for the analysis of glycerol dialkyl glycerols tetraethers (GDGTs) that may be used to determine the TEX86 palaeotemperature proxy. The UK palaeoenvironmental community would benefit greatly by the provision of this analytical service for which the node will utilise triple quadrupole LC/MS instrument bought utilising funds secured through the 2007/2008 capital funding round. Our current aim is to have this as a routine technique by the autumn application deadline. The second methodology to be developed will be various techniques employing the use of a recently acquired ThermoFisher Scientific ISOLink interface for the isotopic analysis of highly polar (amino acids, monosaccharides) and macromolecular compounds (proteins, DNA). Once tested and proven robust these methodologies will be offered as a unique, new service to users of NERC LSMSF. Non-Mandatory Facility-specific OPMs: utilisation, allocation of capacity etc See separate Annexes.