SERVICES & FACILITIES ANNUAL REPORT - FY April 2007 to March 2008
SERVICE Open University Uranium
Series Facility
FUNDING
block
AGREEMENT
F14/G6/47
ESTABLISHED as S&F
1998
TERM
3
TYPE OF SERVICE PROVIDED:
The purpose of the Open University Uranium-Series Facility (OUUSF) is the application of U-series
methodologies in research in Earth and environmental sciences and science-based archaeology. Research
projects are carried out, subject to approval by the Steering Committee, in collaboration with NERC
stakeholders in the pursuit of knowledge and better understanding of the Earth system. U-series chronology is
an essential component of many projects in Earth and environmental science, oceanography, hydrology and
science-based archaeology. Current OUUSF research includes projects on global climatic change through
dating of authigenic deposits, human evolution, magma evolution and volcanic hazard prediction, and
sedimentation rates. Uranium-series determinations, e.g. 234U/238U, 230Th/232Th, 231Pa/235U 230Th/234U ratios,
and U, Th Pa and Ra concentrations by isotope dilution, are performed on a dedicated TIMS MAT262-RPQ-II
instrument or a Nu Instruments MC-ICPMS. Both are equipped with a deceleration lens to achieve the required
abundance sensitivity, and ion counting for superior detection statistics. Thorium isotope ratios in samples
containing less then 0.5 picogram 230Th can be measured with a precision better than 1% (2m) and Ra
abundances, as low as 4 femtogram, can be determined to 1% (2m). OUUSF uses Picotrace state-of-the-art
ultra-clean chemical laboratories for sample separation and purification. Low total procedure blanks and
excellent instrument sensitivity provide the means to analyse very low level abundances in samples, for
instance Ra in mid-ocean ridge basalts and Th dissolved in water.
OUUSF provides the equivalent of one user-year of training and analyses per annum, which represents
25% of the Open University Isotope Geochemistry Laboratory capacity and corresponds to circa 165
samples. Post-graduate teaching and training is the most important aspect of OUUSF activity and usually
post-graduates work under close supervision in the laboratory for a number of short periods. Students use
Standard Operating Procedures and learn to work with radioactive materials in a low-blank chemistry
laboratory, a mass spectrometry laboratory and to carry out data reduction and evaluation protocols.
Quality Assurance is maintained through the repeated analysis of internal laboratory standards and
Certified Reference Materials, reagent and total-procedure blanks and calibrations, performed by staff and
users, equivalent to some 30 samples per year. OUUSF staff has some capacity to perform analyses for
collaborators.
Scientific results of collaborative research may be included in PhD thesis, published in scientific journals,
presented at conferences or disseminated in electronic media.
OUUSF has an extensive web-site URL: http://www2.open.ac.uk/ou-usf/
ANNUAL TARGETS AND PROGRESS TOWARDS THEM
The OUUSF Agreement provides for the equivalent of 165 analyses, equating to 25% of capacity and this has
been achieved. Most data were communicated to the PI within the timeframe of the project.
SCORES AT LAST REVIEW (each out of 5)
Need
Uniqueness
CAPACITY of HOST ENTITY
FUNDED by S&F
25 %
Quality of Service
Date of Last Review:
Quality of Science & Training
Staff & Status
Dr P van Calsteren, Senior Research Fellow: 48%
Dr L E Thomas, Project Officer: 100%
Mr M Davies, Grade 6 technician: 50%
FINANCIAL DETAILS: CURRENT FY
Total Resource
Unit Cost £k
Allocation
Unit 1
Unit 2
Unit 3
£k
166.86
868.65
FINANCIAL COMMITMENT (by year until end of current agreement) £k
2007-08 143.36
2008-09 147.98
2009-10 152.42
2010-11
STEERING COMMITTEE
NIGFSC
Independent Members
7, (chair Prof S Metcalfe)
Meetings per annum
2
Average
Next
Review
(January)
2010
Capital
Expend £k
Income
£k
23.5
0
157.00
2011-2012
Other S&F Overseen
NIGL, AIF, ICSF
Contract
Ends
(31 March)
2011
Full
Cash
Cost £k
143.36
APPLICATIONS: DISTRIBUTION OF GRADES (Current FY — 2007/08)
R*/Pilot
5
4
3
2
1

NERC Grant projects
Other academic
Students
3
Pilot
3
TOTAL
APPLICATIONS: DISTRIBUTION OF GRADES (per annum average previous 3 years —2004/2005, 2005/2006 & 2006/2007)
R*/Pilot
5
4
3
2
1

NERC Grant projects
.33
1.33
.67
Other Academic
.33
1.67
.33
Students
1.33
.33
Pilot
.33
.33
3.33
2
1
TOTAL
Reject
Reject
PROJECTS COMPLETED (Current FY)
5
4
NERC Grant projects
Other Academic
Students
Pilot
3
3
1
1
1
2
1
Grand
Total
3
2
2
Other
1
NERC
Grant*
NERC
Grant*
*Combined non-Directed and Directed
PAYG
Student
NERC
Other
C/S
NERC Other
1
USER PROFILE (per annum average previous 3 years)
Infrastructure
Grand
Student
Total
Supplement to NERC Grant *
NERC Other
5
1.67
1.67
1.33
USER PROFILE (current FY)
Academic
Centre/Survey
3
USER PROFILE (per annum average previous 3 years)
Academic
Centre/Survey
5
NERC
C/S
NERC
C/S
Other
2.33
NERC Fellows
PhD
Commercial
NERC Fellows
PhD
Commercial
OUTPUT & PERFORMANCE MEASURES (current FY)
Publications (by science area & type)
SBA
ES
MS
AS
TFS
EO
Polar
Grand Total
Refereed
3
3
3
Distribution of Projects (by science areas)
SBA
ES
MS
AS
TFS
3
OUTPUT & PERFORMANCE MEASURES (per annum average previous 3 years)
Publications (by science area & type)
SBA
ES
MS
AS
TFS
EO
Polar
Grand Total
Refereed
.67
3
3.67
SBA
.33
ES
2
R*/Pilot
*Combined non-Directed and Directed
PAYG
Student
NERC
Other
C/S
NERC Other
USER PROFILE (current FY)
Infrastructure
Student
Supplement to NERC Grant *
NERC Other

Distribution of Projects (by science areas)
MS
AS
TFS
Non-Ref/ Conf Proc
EO
Non-Ref/ Conf Proc
EO
PhD Theses
Polar
PhD Theses
Polar
Distribution of Projects (by old NERC strategic priority) (as whole or part of whole number NOT as a %)
Earth’s life support systems
Climate Change
Sustainable Economies
Underpinning Science
Specific Research
14
1
Distribution of Projects (by new NERC strategic priority) (as whole or part of whole number NOT as a %)
Climate System
3
Biodiversity
Earth System Science
Sustainable Use of
Natural Resources
Natural Hazards
Environment, Pollution
& Human Health
Technologies
YES
OVERVIEW & ACTIVITIES IN FINANCIAL YEAR (2007/08):
This year was the ‘sunsetting’ period to bring approved projects to a proper ending after the negative judgement by
SRG in the 2006 review. During this period, no new projects were considered for approval but 3 projects were submitted
to NIGFSC after consultation with the NERC S&F Office. The 3 projects comprised one where PGRS hardship would
have resulted and the invited resubmissions of a project first assessed by NIGFSC in 2006. All 3 are PGRS projects and
attracted 3h grades
In 2007, a baseline review by SRG recommended a more focused review of the facilities which support Isotope
Geosciences. A review panel, NIGFR, was set up and one of the recommendations was an assessment of demand for
continued provision of a U-series facility. This case was made and tenders were invited. The Open University U-series
Facility bid included many letters of support from its collaborators and was ranked first in this tendering exercise. NERC
S&F and The Open University have agreed that OUUSF will be funded for a further 3 year from April 2008.
The MAT262 mass spectrometer has been performing well, with a further short interruption when the mains power
distribution unit malfunctioned and was repaired (under warranty). The Nu Instruments MC-ICPMS performed well and
is used mainly for low abundance Th measurements when higher sensitivity is more important than better precision.
The new Thermo-Finnigan Neptune MC-ICPMS has been extensively tested for U-series analyses using the same
standards as are analysed routinely on the Nu Instruments MC-ICPMS. The RPQ-SEM detector systems are very similar
on both instruments but the Neptune has a triple channeltron detector where the Nu has 3 discrete dynode SEMs.
Standard solutions, including simple dilutions of established CRMs or of our own ‘tailored’ mixtures, such as the widely
analysed Th’U’std, as well as ‘bespoke’ mixtures of isotope ratio standards with spikes were analysed in routine
operating conditions. The results are such that for our mode of operation there are no significant differences in sensitivity,
accuracy and precision between the two instruments. Based on these results, it has been agreed within the Department to
largely dedicate the Nu Instruments MC-ICPMS to U-series analysis and to give its management to OUUSF staff.
A 50% contribution from NERC S&F has allowed the purchase of a gamma spectrometry setup for the confident
tracking of 237Np and 233Pa through our chemical separation procedure for 231Pa quantification. The instrument
components have been delivered in March 2008 for installation and commissioning in April/May 2008.
The OUUSF website has been kept up-to-date and has an Introduction into Uranium-series methodology, examples of
Projects, lists of Publications and links to the laboratory Risk Assessments. For laboratory users there are also links to all
Standard Operating Procedures and Training Manuals, as well as spreadsheets and compilations of our laboratory
standards and blanks. The intention of this e-documentation is to comply with the spirit of ISO:9001 Quality Assurance
by Quality Control at a day-to-day level and by evaluation of QC data.
19 ‘rock’ standards were analysed as unknowns, as well as 86 total procedure blanks, reagent blanks and shelf
standards traceable to Certified Reference Materials to maintain high levels of Quality Control. On the MC-ICPMS 186
traceable standards were analysed in Sample-Standard analysis protocols.
Since 2004 there were 15 active projects, of which 6 were finished in 2007. Nine projects form part of a PhD project
and 4 post-graduate received intensive training at the OUUSF laboratory. Three papers involving OUUSF staff or data
were published in peer-reviewed journals, 3 have been submitted.
Papers published (numbers since 1998):
33. Marshall, J.D., Weedon, G.P., Lang, B., Kiriakoulakis, K., Fisher, E.H., Crowley, S.F., Ball, J.D., Jones, R,T.,
Calsteren, P. van, Bedford, A., Brooks, S,J., Muscheler, R., Johnsen, S. (2007). Early Holocene climate in NW
Europe - abrupt events, centennial variability, and solar influence. Geology, 35( 7), 639–642. (IP/672/0900) GC
34. Asrat, A., Baker, A., Umer, M., Leng, M.J., van Calsteren, P. and Smith, C.L., 2007. A high-resolution multi-proxy
stalagmite record from Mechara, Southeastern Ethiopia: Paleohydrological implications for speleothem paleoclimate
reconstruction. Journal of Quaternary Science, 22, 53-63. (IP/932/1106) GC
35. Caseldine, C.J., McGarry, S.F., Baker, A., Hawkesworth, C. and Smart, P.L. 2008. Late Quaternary speleothem
pollen in the British Isles. Journal of Quaternary Science, DOI: 10.1002/jqs.1121. (IP/578/0998) GC
SCIENCE HIGHLIGHTS
Science highlight of 2007 was the publication of Caseldine, C. J., McGarry, S. F., et al., Quaternary speleothem
pollen in the British Isles. J. Quaternary Sci., (2007), ISSN 0267-8179, partly based on McGarry’s thesis research at
OUUSF on dating stalagmite samples. This paper has attracted much praise from the palaeo-anthropology community.
Stalagmites offer a significant advantage over many other sources of palaeo-environmental information because they
can be dated with high precision and accuracy by the 234U-230Th method and they can contain sufficient well-preserved
pollen from contemporaneous vegetation above the cave to allow palaeo-environmental reconstruction. In samples from
Lancaster Hole and Stump Cross Caverns in the Yorkshire Dales and Holcombe Quarry Cave in the Mendip Hill, the
presence of thermophilous vegetation, including trees, has been demonstrated through the analysis of pollen, indicating
that the climate was fairly
equitable. U-series ages
Speleothem ages
show that temperate
20
periods occurred in Britain
during interstadials within
0
the Last Glaciation, in
20
40
60
80
100
120
particular during MIS 5c,
warm:
3333333333333333333
5a5a5a
5c5c5c
5e5e5e5e5e
5a, 4 and 3, (see figure).
The 18O graph is a proxy
-34
for ice volume/sealevel.
-36
Ages of Individual D/O
oscillations within
-38
interstadials are determined
-40
by interpolation rather than
by independent dating. It is
-42
not feasible to pinpoint a
-44
‘cool’ or ‘temperate’ part
of a D/O oscillation
-46
Whiskers indicate U-series ages (±uncertainty) for stalagmite
18
because the actual duration
samples with ~20% thermophile pollen (Caseldine et al., 2007)
 O
18
Blue line indicates  O variations in Greenland ice-core (NGRIP, 2004)
is uncertain. Correlations
with the late Pleistocene
biostratigraphy of the British Isles are hampered by the incomplete nature of the deposits, and the lack of well-dated
records. However, it is clear that locally at least, climate conditions were less extreme than usually accepted (see: Lowe
and Walker, 1997 for an overview).
White (2006) has pointed out that the lack of wood to be used as hafts for tools or weapons and for fire, would have
made it very unlikely that conditions were sufficient for survival of Neanderthals during cool episode. However, the
presence of trees, albeit possibly restricted to sheltered valleys, over a wide age range of the British Isles, may have been
the crucial factor that allowed Neanderthals colonisation, albeit maybe only for short periods.
% thermophile
FUTURE DEVELOPMENTS/STRATEGIC FORWARD LOOK
Analytical developments: The performance of the MAT262-RPQ-II instrument for U-series analysis, mainly by ion
counting, is on a par with more modern Thermal Ionisation Mass Spectrometers and in ‘total evaporation’ mode with the
ultra-fast GPIB voltmeter, outperforms modern instruments for very small samples. The Nu Instruments plasma
ionisation mass spectrometer (MC-ICP-MS) now has fully developed protocols for U-series analyses and is used where
sensitivity is of prime importance. TIMS is used when mass-dependent isotope fractionation and instrument drift, which
are both an order of magnitude better, is a requirement for high precision (for high resolution) and when concentration or
availability are not limiting factors. For Radium the sensitivity of TIMS is easily a factor of 20 better then MC-ICP-MS,
and TIMS remains the instrument of choice.
The U-series-dedicated channeltron configuration on the Neptune has similar sensitivity and precision as the discrete
dynode ion multipliers (DDIM) on the Nu Instruments. However, the channeltron detectors show significantly more drift
as the DDIM on the Nu. We analyse 234U and 236U on channeltrons on either side of a 235U in a Faraday collector with a
1012  resistor. Ratio drift correlates with accumulated beam charge (Coulomb) in the channeltrons to the extent that the
235
U/236U ratio drifts substantially faster than the 234U/236U ratio. Ratio drift is such that calibration is not practical but
good results have been obtained with the Standard-Sample-Standard analysis strategy. However, improvement in
analytical statistics relative to the performance of the Nu Instruments is not significant.
Either MC-ICPMS can be hyphenated to the Excimer laser ablation system but samples with sufficient U
concentration and age, other than coral, to explore the potential of this technique are fairly rare.
OUUSF is continuing the implementation of mass spectrometric analysis of 231Pa. Radioactive Risk Assessment, in
particular regarding the 237Np precursor of the 233Pa spike, required the purchase of a dedicated gamma spectrometer, in
addition to the  and  monitors. When commissioned in April/May 2008 the gamma spectrometer will greatly benefit the
fine tuning of the Pa chemical preparation protocols. Mass spectrometry procedures are now in place and further experience
with this method will lead to further streamlining and improvements.
Strategic look forward: The new arrangement where OUUSF staff manages both the MAT262 TIMS and the Nu
Instruments MC-ICPMS means faster sample throughput and project turn-around time for the future.
Incorporation of the gamma spectrometer into our routine operations is an important strategic goal, not only to
improve our performance with 231Pa analysis but also to streamline 226Ra and 229Th spiked procedures
We plan to better promote the U-series facility in the wider academic community and we are taking part in ‘Outreach’
activities where we are setting up an interactive display about uranium in the environment. Both LET and PvC are trained
as Science and Engineering Ambassadors.
Non-Mandatory Facility-specific OPMs: utilisation, allocation of capacity etc
OUUSF Mission Statement
 OUUSF is hosted by the Isotope Geochemistry Research Group, Earth and Environmental Sciences, The Open
University.
 OUUSF is providing U-series methodology through collaborative projects to researchers within the NERC remit
to further the goals in NERC strategy 2007-2012: Next generation science for planet Earth, Science-based
Archaeology and responsive mode (‘blue skies’) research.
 OUUSF provides web-based training material and one-to-one training for post-graduates and research scientists
in U-series laboratory techniques, underlying theory and data evaluation.
 OUUSF pursues an ‘open door’ attitude and will share methods and protocols with collaborators and the wider
scientific community.
 OUUSF aims to expand and improve analytical techniques for chemical preparation in a state-of-the-art
laboratory, using the latest mass spectrometric instrumentation, to support innovative collaborative projects.
NERC Isotope Geoscience Facilities Steering Committee, 2008
Chair: Prof. Sarah Metcalfe
School of Geography
University of Nottingham
Nottingham, NG7 2RD
Tel: +44 (0) 115 8467712
E-mail: sarah.metcalfe@nottingham.ac.uk
Members:
Prof Julian E Andrews
School of Environmental Sciences
University of East Anglia
Norwich, NR4 7TJ
Tel: 0160 359 2536
E-mail: j.andrews@uea.ac.uk mailto:j.andrews@uea.ac.uk
Prof SA Bowring
Department of earth, Atmospheric, and Planetary Sciences
MIT Building 54-1126
Cambridge, MA 02139 USA
Tel: +10617 2530 3775
E-mail: sbowring@mit.edu
Prof. Colin Graham
School of GeoSciences
The University of Edinburgh
Grant Institute
The King's Buildings
West Mains Road
EDINBURGH EH9 3JW
Tel: 0131 650 4849
E-mail: Colin.Graham@ed.ac.uk
Dr RA Mills
School of Ocean and Earth Sciences
National Oceanography Centre, Southampton
Southampton, SO14 3ZH
Tel: 023 8059 2678
E-mail: ram1'noc.soton.ac.uk
Prof Clive M Rice
College of Physical Science
School of Geosciences
Secretary: Béatrice Bullock-von Moos
NERC Isotope Geosciences Laboratory
British Geological Survey
Kingsley Dunham Centre
Keyworth, NG12 5GG
Tel. 0115 / 936 3425
Switchboard 0115 / 936 3100
bbullock@bgs.ac.uk
Ex-officio:
Dr Adrian J Boyce
SUERC
Rankine Avenue
East Kilbride
Glasgow, G75 0QU
Tel: 01355 270143
E-mail: a.boyce@suerc.gla.ac.uk
Dr Fin M Stuart
SUERC
Rankine Avenue
East Kilbride
Glasgow, G75 0QU
Tel: 01355 270139
E-mail: f.stuart@suerc.gla.ac.uk
Dr R Lin F Kay
Science and Innovation Funding
NERC
Polaris House
North Star Avenue
Swindon, SN2 1EU
Tel: 0179 341 1500
E-mail: rlfk@nerc.ac.uk
Prof. Melanie J Leng
NERC Isotope Geosciences Laboratory
British Geological Survey
Kingsley Dunham Centre
Keyworth
Nottingham, NG12 5GG
Tel: +44 (0) 115 936 3515
Geology & Petroleum Geology
Meston Building
King’s College
Aberdeen, AB24 3UE
Tel: +44 (0) 1224 273433
E-mail: c.rice@abdn.ac.uk
Prof. K Thomas
University College London
Institute of Archaeology
31-34 Gordon square
London, WC1H 0PY
Tel: 0207 6794 767
E-mail: k.thomas@ucl.ac.uk
Prof Jim Marshall
Earth and Ocean Sciences,
University of Liverpool
Tel:(+44) (0)1517945177
E-mail: isotopes@liv.ac.uk
Fax: +44 (0) 115 936 3302
E-mail: mjl@nigl.nerc.ac.uk
Prof. Randy R Parrish
NERC Isotope Geosciences Laboratory
British Geological Survey
Kingsley Dunham Centre
Keyworth
Nottingham, NG12 5GG
Tel: 0115 936 3427
E-mail: r.parrish@nigl.nerc.ac.uk
Dr Peter van Calsteren
Department of Earth Sciences
The Open University
Walton Hall
Milton Keynes, MK7 6AA
Tel: 0190 865 2889/655151
E-mail: p.v.calsteren@open.ac.uk
Dr S Davies
Room E21d, Institute of Geography and Earth Sciences,
Llandinam Building
Penglais Campus, Aberystwyth
Ceredigion SY23 3DB, Wales, UK
Tel: (01970) 622585
E-mail: sjd@aber.ac.uk
NIGF Steering Committee: Remit
The NERC Isotope Geosciences Facilities Steering Committee exists to:
review applications for use of:
the NERC Isotope Geosciences Laboratory;
the Argon Isotope Facility at the SUERC;
the Isotope Community Support Facility at the SUERC; and
the Open University Uranium Series Facility
monitor outputs from these Facilities;
provide advice to the Director, Science and Innovation Funding on aspects of the operations of these Facilities.
The Director, Science and Innovation Funding, in turn, provides advice to the Science and Technology Board of
Council on Services and Facilities relevant to their remit.
Terms of Reference
1. To review applications and to establish priorities for the Heads of these Facilities in the allocation of those of the
Facilities’ resources funded from the Science and Innovation Funding allocation, taking into account NERC
Strategy and recommendations made through the NERC peer-review mechanisms.
2. To review the scientific quality of work undertaken by users utilising these Facilities, based on reports and
publications.
3. To monitor the level of user-satisfaction with the Facilities, and to analyse the user-base.
4. To give guidance to the Heads of these Facilities on improvement of the Facilities’ equipment and on their service
function.
5. To advise the Director, Science and Innovation Funding on:
5.1. the level and direction of the internal R & D programme for these Facilities;
5.2. the anticipated levels of future demand and any consequential anticipated changes in resource requirements
from these Facilities.
5.3. on other matters, as appropriate and reasonable.
6. To receive annually a report from the Heads of these Facilities, and comment through the Chair on them before
passing them to the Director, Science and Innovation Funding.
1. Equipment Inventory
OUUSF does not own any equipment
2. Future Developments.
In situ analysis:
The sensitivity of our MC-ICPMS is such that it is be possible to measure (234U/238U) and (230Th/232Th)
in situ in coral samples using the NewWave-193 UV excimer laser ablation system. The technique has
important applications in marine climate change studies. The energy of the laser at the ablation point is such
that a short-lived Laser-Induced Plasma is produced and this adds another process by which mass and
element fractionation takes place. The use of appropriate coral standards is essential and it is not simple to
find a suitable standard that is homogeneous at the spatial resolution that is required. However, age variation
patterns are much easier to resolve and this is frequently the main purpose.
Protactium and Radium
OUUSF now has methods for mass spectrometric analysis of 231Pa, the daughter of 235U with a half-life
of ~35,000 y. All necessary Radioactive Risk Assessments, including the 237Np precursor of the 233Pa spike,
have been completed and approved. An analytical method to purify protactinium from silicate rocks was
published recently (Regelous et al., 2004), but this has required extensive variations for the chemical
separation of protactinium from carbonate-rich samples.
The newly purchased gamma spectrometry system will be fully commissioned in April/May 2008 and
gamma spectrometry will make it possible to ‘track’ spiked samples through the chemical separation
procedure. Adjustments can then be made to the procedure to improve sample recovery. However, the
main reason for gamma spectrometry is the advice from the University Radiation Safety Advisor that we
should develop the ability to not only simply track radioactivity but to identify the nuclide that is the main
reason for the detected radioactivity.
231
Pa dating can provide confirmation of ages obtained by 230Th dating. Two independent estimates of
the age from the same sample would be useful for dating of speleothem carbonate and particularly in
archaeological bone using the Oxford U-uptake model (Millard and Hedges, 1996), recently further
developed for U-series (see Pike et al., 2002).
231
Pa has found application in coral dating (Mortlock et al., 2005, Edwards et al., 1997). In open
oceans, 231Pa and 230Th are removed from the water column by a process of reversible scavenging (Moran
et al., 2002, Moran et al., 2005) which quickly removes 230Th to the sediment. 231Pa is less efficiently
scavenged onto particles than 230Th and is therefore more effectively transported via advection and
diffusion before it reaches the ocean sediment. The equilibrium partition coefficients for particulate versus
dissolved matter may vary with particle type and the (231Pa / 230Th) activity ratio can be of great use in
paleo-oceanographic studies.
231
Pa/235U data will also be useful in future projects on young volcanics and will form part of the
already approved project on Axial Volcanic Ridges. The sampling cruise will take place in May/June 2009
and PvC will join the ship-board scientific party.
The U-series sub-system 230Th-226Ra has a half-life of 1602y which makes it highly appropriate for
systems with millennial ages. Using TIMS with ion counting we can analyse <4 femtogram 226Ra routinely
and this is essential because 226Ra is present at the femtogram/gram level in geological materials. The age
of a sample is calculated from the 226Ra/Ba ratio in the sample relative to present day 226Ra/Ba. The
uncertainty in 226Ra/Ba ages depends mostly on the assumption that 226Ra/Ba has remained constant. This
is a reasonable assumption because Ra and Ba have very similar geochemical characteristics. TIMS 226Ra
dating has never previously been applied to speleothem samples and an application in conjunction with
lamina counting that would re-enforce confidence in both methods and confirm the validity of the 226Ra/Ba
dating method in young authigenic carbonates in Holocene speleothems, is being developed.
Authigenic minerals precipitates from groundwater.
Long-standing assumptions in U-series dating of authigenic minerals are that all accumulated 230Th is
from in-situ decay of 234Uand only U and no Th is transported in ground water. The concentration of trace
elements in water is determined by temperature, pH, redox conditions, concentration of anionic ligands and
complex ions formation. Residence time in groundwater is a function of the rate of leaching, stability of
complex ions, and adsorption onto particulate matter or incorporation into authigenic minerals. The
resulting U/Th in groundwater is usually > 10,000.
Contrary to expectations, recent work at The Open University has shown that Th and U have similar
concentrations in oxygenated ground water in the Great Artesian Basin, Australia. It is likely that U and Th
speciation is the determining factor for this unexpected behaviour and furthermore this makes the longstanding U-series dating assumptions questionable. Any 230Th that is not derived from in-situ decay but is
transported in ground water must therefore be accounted for before meaningful ages can be calculated.
The theoretical framework for the behaviour of U and Th in ground water can now be tested due to
recent advances in analytical technology. These recent advances allow the speciation of U and Th to be
determined at the low concentration levels encountered in groundwater.
To assess the effects of 230Th transportability in groundwater is is necessary to:
1. determine the speciation of U and Th isotopes in groundwater;
2. develop a thermodynamic framework for the speciations;
3. evaluate the importance of these findings for U-series dating of authigenic minerals.
Our new generation ThermoFinnigan Neptune (SM-ICPMS) with multi-channeltron ion counting is be able
to measure pico-gram quantities of analyte purified by hyphenated High-Performance LiquidChromatography (HPLC).
3. Summary of Performance Information
Projects active in 2007/2008
Grade
allocation
analysed 2007
ENRI
15
ES
GC
a4m
61
6
P
Acad collaboration
ES
GC
a4l
30
NT
P
Acad collaboration
ES
CS
a4m
15
20
J
NT
P
Acad collaboration
SBA
a4l
24
14
RA
NT
P
Acad collaboration
ES
CS
a4h
15
15
prof
RC
NT
P
NE/C5205981/1
ES
CS
R*
Baker
dr
A
NT
P
S
Acad collaboration
ES
CS
a4m
10
11
Thomas
prof
D
NT
P
S
NER/S/A/2005/13353
ES
CS
a3h
50
16
Geography
Lawson
dr
IT
NT
P
Acad collaboration
ES
CS
a4h
24
SES
Andrews
prof
J
NT
P
NER/A/2005/13582
ES
CS
a3h
18
IP/864/0505
H-0073
Plymouth
Geography
Roberts
prof
CN
NT
P
2005
IP/865/0505
H-0121
Keele
School ES&G
Gertisser
dr
R
NT
P
live
48
2005
IP/867/1105
H-0126
Liverpool
E&O science
Marshall
prof
J
NT
P
live
50
2005
IP/878/1105
H-0204
Manchester
Geography
Woodward
dr
J
NT
live
51
2006
IP/906/0506
H-0155
Nottingham
Geography
Metcalfe
prof
S
live
53
2006
IP/911/0506
H-0112
Bristol
Archaeology
Zilhao
prof
live
54
2006
IP/912/0506
H-0160
Southampton
SOES,NOC,S
Mills
dr
live
55
2006
IP/929/1106
H-0116
Durham
Earth Sciences
Searle
done
56
2006
IP/932/1106
H-0110
Birmingham
SGEES
live
57
2006
IP/937/1106
H-0156
Oxford
OUCE
live
58
2006
IP/938/1106
H-0124
Leeds
done
59
2006
IP/939/1106
H-0117
UEA
PI initials
2005
47
University
Sience area
15
NER/A/S/2002/00885
Type
50
a4m
46
done
HERA
Student
a4l
GC
Mode
GC
ES
PI title
ES
Acad collaboration
PI name
Acad collaboration
live
IP number
Institute
S
S
S
S
18
done
60
2007
IP/961/0507
H-0117
UEA
SES
Leeder
prof
M
NT
P
S
Acad collaboration
ES
CS
a3h
10
12
done
61
2007
IP/977/0507
H-0117
UEA
SES
Andrews
prof
J
NT
P
S
NER/A/2005/13582
ES
CS
a3h
16
16
done
62
2007
IP/998/1107
H-0117
UEA
SES
Andrews
prof
J
NT
P
S
NER/A/2005/13582
ES
CS
a3h
10
10
SC
63
2008
IP/1025/0508
H-0117
UEA
SES
Andrews
prof
J
NT
P
Acad collaboration
ES
ESS
SC
64
2008
IP/1032/0508
H-0116
Durham
Earth Sciences
Armstrong
dr
H
NT
P
NER/S/A/2005/13868
ES
ESS
SC
65
2008
IP/1049/0508
H-0114
Cambridge
McDonald Inst
Rabett
dr
R
NT
P
Acad collaboration
SBA
CS
S
4. Publication details, numbers since 1998, IP code and Science Area.
Papers published in 2005:
36. Zellmer G.F., Annen, C., Charlier, B.L.A., George, R.M.M., Turner, S.P., Hawkesworth, C.J. (2005) Magma
evolution and ascent at volcanic arcs: constraining petrogenetic processes through rates and chronologies.
Journal of Volcanology and Geothermal Research 140, 171-191. (IP/633/0999) ES
37. Pike, A.W.G., Eggins, S. Grun,R., Hedges, R.E.M., Jacobi, R.M.(2005) U-series dating of the Late Pleistocene
mammalian fauna from Wood Quarry (Steetley), Nottinghamshire, UK. Journal of Quaternary Science 20(1),
59–65. (IP/654/0300) SBA
38. Pike, A.W.G., Gilmour, M., Pettitt, P., Jacobi, R., Ripoll, S., Bahn, P., Munoz, F. (2005) Verification of the age
of the Palaeolithic cave art at Creswell Crags, UK. Journal of Archaeological Science 32, 1649-1655.
(IP/654/0300) SBA
Papers published in 2006
39. Thomson, J., Green, D.R., Calsteren, P. van, Richter, T.O., Weering, T.C.E. van. (2006,). Holocene sediment
deposition on a NE Atlantic transect including Feni Drift quantified by radiocarbon and 230Thexcess methods.
Earth and Planetary Science Letters, 242, 170-185. (IP/791/1103) ES
40. Hughes, P.D., Woodward, J.C., Gibbard, P.L., Macklin, M.G., Gilmour, M.A. and Smith, G.R. (2006), The
Glacial History of the Pindus Mountains, Greece, Journal of Geology 114, 413–434. (IP/754/0302) GC
41. Hughes, P.D., Gibbart, P.L.and Woodward, J.C. (2006), Middle Pleistocene glacier behaviour in the
Mediterranean: sedimentological evidence from the Pindus Mountains, Greece. Journal of the Geological
Society, London, 163, 857–867. (IP/754/0302) GC
42. Hughes, P.D., Woodward, J.C. and Gibbard, P.L.(2006) Late Pleistocene glaciers and climate in the
Mediterranean region. Global and Planetary Change, 46, 83-98. (IP/754/0302) GC
43. Hughes, P.D., Woodward, J.C. and Gibbard, P.L. (2007) Middle Pleistocene cold stage climates in the
Mediterranean: new evidence from the glacial record. Earth and Planetary Science Letters,253(1-2), 50-56.
(IP/754/0302) GC
Papers published in 2007-8
44. Marshall, J.D., Weedon, G.P., Lang, B., Kiriakoulakis, K., Fisher, E.H., Crowley, S.F., Ball, J.D., Jones, R,T.,
Calsteren, P. van, Bedford, A., Brooks, S,J., Muscheler, R., Johnsen, S. (2007). Early Holocene climate in NW
Europe - abrupt events, centennial variability, and solar influence. Geology, 35( 7), 639–642. (IP/672/0900) GC
45. Asrat, A., Baker, A., Umer, M., Leng, M.J., van Calsteren, P. and Smith, C.L., 2007. A high-resolution multiproxy stalagmite record from Mechara, Southeastern Ethiopia: Paleohydrological implications for speleothem
paleoclimate reconstruction. Journal of Quaternary Science, 22, 53-63. (IP/932/1106) GC
46. Caseldine, C.J., McGarry, S.F., Baker, A., Hawkesworth, C. and Smart, P.L. 2008. Late Quaternary speleothem
pollen in the British Isles. Journal of Quaternary Science, DOI: 10.1002/jqs.1121. (IP/578/0998) GC
Targets & Milestones

instrument utilisation;
The OUUSF Agreement is for the utilisation of 25% of the U-series laboratory capacity, equivalent to
approximately 165 samples per year and this target has been achieved. 19 ‘rock’ standards were analysed as
unknowns to assess the full analytical protocol. 86 Total procedure blanks, reagent blanks and shelf standards
traceable to Certified Reference Materials were analysed to monitor routine performance for Quality Control
purposes in the spirit of ISO:9001. On the MC-ICPMS 186 traceable standards were analysed in Sample-StandardStandard analysis protocols. Dozens of test solutions were devised and tested as part of the 231Pa analysis protocol
developments

allocation of capacity and effort;
Instrument and laboratory time for OUUSF operations were scheduled in consultation with other users and
there was no friction.

throughput;
The analytical workload in the ‘sunsetting’ year has been significantly above average and our usual turnaround times have not always been maintained.

response times and data delivery to customers;
Analytical results have mostly been submitted to PI’s within the agreed time-frame with a few exceptions.
‘Teething trouble’ with the protactinium method and the large number of samples for which a ‘detrital’
correction is required, have resulted in delays. Communications regarding interpretations and publication
are always conducted with the highest priority.

user satisfaction;
In response to a request for a letter of support to our existing collaborators resulted in a large number of
universally highly supportive responses. These were included with the OUUSF bid and have no doubt
contributed to the decision to award a new Facility Agreement. Details of the complaints procedure are on
the OUUSF website; no complaints were made.

scheduled maintenance, calibrations, planned contingency, down time due to external factors
etc.;
The MAT262 has been out of action for a week to fix a residual problem with the mains distribution unit,
but schedules were recovered very soon afterwards.

summary of internal R&D output;
New models have been developed and tested to interpret U-series data. This includes a mixing model to
assess and correct for allogenic 230Th components for moderate contributions and a simple subtraction
model where that is justified for very small allogenic contributions. In the latter case, simple subtraction is
more appropriate because it avoids propagation of the relatively large uncertainty inherent in the
determination of small amounts of 232Th. A further model has been perfected to evaluate ‘open system’
behaviour and this has been shown to be an effective tool in evaluating data of Namibian tufa samples.
A spreadsheet-based model to evaluate Pa data is still in a quite simple form but should be fully functional
in 2008.
5.
Finance
Details are included in the account filed by the The Open University Finance Division.
6. Service Management
Peter van Calsteren is Principal Investigator and Manager of OUUSF as Senior Research Fellow in the
Faculty of Science at The Open University. Louise Thomas is Project Officer and is OUUSF-funded
through the NERC-OU Agreement. Dela Fazel was Part-Time (50%) Grade 6 Technician, OUUSF-funded
through the NERC-OU Agreement till 31 December 2007. Dela has accepted an appointment as Course
Manager at the OU and Marc Davies, an OU PGRS has taken over till the end of April 2008. Recruitment
is in progress for a grade 6 technician, hopefully for the full term of the Agreement. A short-list has been
drawn up from a list of 10 applicants, interviews will be on 1 May 2008. All OUUSF staff are employed by
The Open University on its standard Terms and Conditions.
7. Projects for which the analytical work has been completed
OUUSF # 44 NIGFSC # IP/862/0505 PI: Dr I Candy Affiliation: Loughborough, Geography Title: A
new approach to Quaternary terrestrial chronologies: U-series dating of earthworm calcite Location: UK
Quarternary Sample type: earthworm granules, Student: N/A, Academic collaboration Grade: 5
Allocation: 10 Analysed: 19
Beyond the timescale of radiocarbon very little exists in the form of absolute chronologies for Quaternary
terrestrial sequences. The aim of the project was to evaluate the potential of dating earthworm calcite by Useries techniques. These calcite granules, formed in the gut of earthworms, are very common in
stratigraphically and archaeologically important sequences and have the potential to provide high
resolution chronologies for both terrestrial response to environmental change and human occupation. For
this pilot study earthworm granules from sites of a range of ages have been analysed. This project did not
quite turn out as expected. The granule materials of which we had only small amounts, were low in
uranium and with Th/U ratios that are normal for silicates, rather than for carbonate, and with high in
radiogenic Th. Such data cannot be modelled to give an age using acceptable assumptions for authigenic
precipitates. It appears that worms are capable of discriminating against U when precipitating the calcite in
the granules in their guts or dissolving U and Th unfractionated from the silicate matrix. Additional
analytical work on recent worms has been carried out to confirm these possibilities and evaluation of these
data by the PI is in progress.
OUUSF # 49 NIGFSC # IP/877/1105 PI: Prof A Baker Affiliation: Birmingham, SGEES Title: Highresolution, multiproxy, multi-stalagmite climate reconstruction from N Turkey Location: NE Turkey
Sample type: stalagmites Student: Cath Jex, Academic collaboration Grade:  4m Allocation: 6
Analysed: 20
PhD studentship funded by SGEES, Phillip Leverhulme Foundation and British Institute at Ankara. The
aim was to reconstruct high resolution climate records from the last 1000 years from annually laminated
stalagmites using a multiproxy approach calibrated against instrumental climate data. Six stalagmites, of
three different morphological ‘species’ that relate to their drip hydrology, have been dated by U-series, as
well as some ‘confirmation’ samples. Cath was trained in the OUUSF lab and carried out the analytical
work in close collaboration with laboratory staff. Cath has submitted her thesis, presented posters at
conferences and is preparing a paper.
OUUSF # 52 NIGFSC # IP/910/0506 PI: Dr M Stokes Affiliation: Plymouth, SEOES Title: Quantifying
mid-late Quaternary landscape response to movements of the Polar Jet Stream in the American west
Location: Jakes Valley, USA Sample type: pedogenic calcrete Student: N/A, Academic collaboration
Grade: pilot- 3h Allocation: 6 Analysed:14
The aim of this project was to date alluvial fans in order to quantify Mid-Late Quaternary climate-related
landscape dynamics within the central Great Basin (American Southwest) to provide a chronology for
climate related rates of soil formation, age estimates of fan lobe abandonment and collectively rates of fan
incision. The relationships of these processes to the pre-Last Glacial Maximum movements of the Polar Jet
Stream should have become clear. The contribution from allogenic silicates was significant, as was
expected. Therefore, 4 sets of 3 closely-related samples were analysed and the data evaluated with the
‘mixing line’ concept (also known as ‘isochron’). Two mixing lines yielded negative slopes that cannot be
interpreted as meaningful ages. Two others did produce ages of 77 Ka and 125 Ka but these ages do not fit
within the established geological framework. Plans to submit a follow-up proposal, or indeed a NERC
Standard Grant application, were abandoned.
OUUSF # 56 NIGFSC # IP/932/1106 PI: Prof A Baker Affiliation: Birmingham, SGEES Title: A
Holocene, high resolution, seasonal rainfall recontruction from Ethiopia Location: Bero, Ethiopia Sample
type: stalagmites Student: N/A Academic collaboration Grade:  4m Allocation: 10 Analysed: 24
Water availability, rather than temperature, is the crucial issue in semi-arid areas, and speleothems in
palaeoclimate studies emphasise the role of climate-triggered hydrological change as being the major
factor driving speleothem proxies in such settings. Improved understanding of the controls of annual
lamina thickness and stable isotopes provides a powerful approach to deriving palaeohydrology, and
characterise the variability of rainfall, which we aim to reconstruct for Ethiopia over the late Holocene
from well characterised stalagmite. U-series dating has confirmed the annual nature of laminae and the
Holocene age of some of the analysed stalagmites. This project is part-funded by the Royal Society and
START. The results of this project have formed the basis of a manuscript that is currently in preparation.
Moreover, the data have formed that basis for a NERC Standard Grant application, which attracted an  4
grade and funding in July 2008
OUUSF # 59 NIGFSC # IP/939/1106, IP/977/0507, IP/998/1107 PI: Prof J Andrews Affiliation: UEA,
SES Title: Palaeoclimatic records from Late Quaternary speleothems in the E Mediterranean
Location:Trabzon Turkey Sample type: stalagmites Student: Jenny Mason, NER/A/2005/13582 Grade:
 3h Allocation: 44 Analysed: 62
Stalagmites from caves in SW and NE Turkey are proxies for recording palaeoclimatic changes during the
Late Quaternary, probably from MIS 5 onward to the Holocene and present. Palaeoclimatic changes have
been recorded principally by stable isotopic data (at UEA) from samples with a well constrained U-series
chronology. This project was seen by NIGFSC on three occasions. Progress was shown, mainly on stable
isotope characterisation of the stalagmites on the second and third submission and more resources were
awarded. Jenny was trained in the OUUSF lab and carried out the analytical work in close collaboration
with laboratory staff, the ‘preliminary’ final total number of ages results from additional effort by Jenny.
The results are incorporated in Jenny’s thesis, to be submitted before the end of the year and she aims to
publish a paper in Science. Her discussions with other authorities in this field, including Myra BarMatthews generated much excitement and a suggestion of maybe a few more dates for the specific purpose
of facilitating comparisons with similar data form the North coast of Turkey by another group in a different
climate zone
OUUSF # 60 NIGFSC # IP/961/0507 PI: Prof M Leeder Affiliation: UEA, SES Title: Sedimentology,
Paleoenvironments and Tectonic significance of Uplifting Marine Terraces in a Forearc Setting, Central
Greece Location: Gulf of Corinth Sample type: Coral Student: Jenni Turner (Smith), Academic
collaboration Grade:  3h Allocation: 10 Analysed: 12
Two distinct uplift models have been proposed in the literature: regional uplift or footwall uplift along
major active on- and off-shore faults. The aim of this PhD project is to test the models by mapping and
establishing chronology of uplifted marine palaeo-shoreline inner edges in key areas. Footwall uplift
should decline with distance (order a few km) from faults, whilst regional uplift should show more general
elevation gradients unrelated to faulting. U-series dating is essential because relative sealevel variations are
caused by both fault-related uplift and actual sealevel variations caused by variations in ice volume.
Cladocora caespitosa coral stems were collected from in-situ coral colonies stratigraphically associated
with possible Holocene, MIS 5 or MIS 7 high-stand mean water levels. Dating of two coral stems from
each in-situ colony is necessary to demonstrate reproducibility of the ages. Five sample sites were selected
as key locations where a chronology will provide the best test for rival models. This proposal was
considered by NIGFSC during the OUUSF ‘sunsetting’ year because the laboratory that was scheduled to
provide the U-series ages for this project could not deliver within the required timeframe. Jenni received
some training but time constraints did were such that she did not carry out her analytical work, but it will
be useful in the next collaborative projects. Jenni has submitted her thesis, has prepared a manuscript and
presented her work at conferences.