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    great analytical facilities!

SAMS' analytical facilities and services

In the pursuit of science excellence, we continue to invest into world-class analytical facilities which support environmental, biological, geochemical, molecular and geological investigations.

These modern instruments support our research projects and education activities but can also be made available for commercial contracts.

For technical enquiries links to individuals working with different instruments are provided.

For commercial enquiries regarding quotes and availability, please contact SRSL: info@srsl.com 

Anyone external interested in using our facilities should contact info@srsl.com. Contact details below are given for anyone requiring more technical information.

Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

The ICP-MS facilities within the department are used for the trace metal analysis of a wide range of sample materials including marine sediments, natural water samples (both fresh and saline), organic tissue and biogenic carbonates such as otoliths. The Thermo Scientific XSeries 2 is a quadrupole ICP-MS fitted with a collision cell to remove problematic oxide interferences. Contact: Dr Richard Abell (E: richard.able@sams.ac.uk)


Inductively Coupled Plasma Mass Spectrometry using Laser Ablation (LA-ICP-MS)

A quadrupole Inductively Coupled Plasma Mass Spectrometer (VG Elemental PlasmaQuad 3 ICP-MS) is coupled to a New Wave UP 213nm solid state Nd:YAG laser. This enables in situ trace metal analysis using either single spots (30 – 750m) or time resolved analysis on a variety of geological and biological samples. Coupling the laser with ICPMS enables trace metal detection limits < 1ng/g (1ppb).

This system is used for the routine measurement of trace metals within biological samples, principally fish otoliths. Ca is monitored as an internal standard, and trace metals abundances normalised to the integrated counts of Ca. External calibration is achieved using the National Institute of Standards glass reference material NIST-612. Contact: Dr Richard Abell (E: richard.abell@sams.ac.uk)


Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)

The Perkin Elmer Optima 4300DV is an ICP-OES instrument capable of multi-element trace metal analysis ranging from low ug/l to g/l levels of concentration. It is utilised to analyse marine sediment samples.

The instrument operates by introducing a sample to the plasma which is ionized Argon gas. The sample is ionized in the plasma causing atoms and ions to emit electromagnetic radiation (light). The emission of light occurs as discrete lines which are separated according to their wavelength by diffractive optics, and are utilised for identification and quantification. The intensity of the light is measured against calibration standards of a known value, allowing for the concentration of the sample to be calculated.

A variety of performance checks, AQC and reference samples are carried out on a per run basis to ensure high quality analysis, and confidence in the results. Contact: Colin Abernethy (E: colin.abernethy@sams.ac.uk)


Piccaro L2130 oxygen isotope mass spectrometer

The isotopic composition of seawater is governed by processes of evaporation, transportation of atmospheric vapor, precipitation and subsequent return of freshwater to the open ocean. In the shelf seas freshwater runoff and ground waters (depleted in 18O) mix with shelf water (enriched in 18O) to define a regional salinity:oxygen isotope relationship.

Precise and accurate analysis of the oxygen isotope composition of seawater can therefore be a powerful tool to differentiate water masses and identify the end members contributing to the formation of water masses.

The Picarro L2130 allows the rapid and high precision measurement of δ18O (<0.025‰, 1σ) and  δ D (<0.1‰, 1σ) of liquid and vapour from marine or meteoric water samples. Contact: Dr Richard Abell (E: richard.abell@sams.ac.uk)


Carbon and Nitrogen Elemental Analyser

Total inorganic carbon and nitrogen (TIC and TIN) and organic carbon (TOC) measurements are performed using a Costech ECS 4010 (Costech Analytical Technologies, CA, USA). This instrument is equipped with a double combustion/reduction furnace for flash combustion and automated simultaneous elemental analysis.

Routine measurement of carbon and nitrogen are performed on a variety of marine samples, such as deep-sea sediments, suspended particulate material, seaweeds and cultured algae. Typically, less than 20mg of material is required to measure sub mg levels of carbon and nitrogen with a precision < 10 %. Accuracy of the instrument is monitored using Chinese National Research Centre, Marine Sediment (GBW-07313 and GBW-07316). In addition to carbon and nitrogen, it is also possible to measure elemental hydrogen, sulphur and oxygen. Contact: Dr Richard Abell (E: richard.abell@sams.ac.uk)


Inorganic Nutrients Autoanalyser

The Lachat 8000 and Lachat 8500 are two flow injection autoanalysers (FIA) capable of measuring the major inorganic algal nutrients, ammonium, phosphate, silicate and nitrate down to 500 nano-molar level. They operate by utilising classical wet chemical reactions to produce colours whose intensity is proportional to the concentration of the nutrient. Detection is then performed by simple flow cell spectrophotometry. Quality assurance is monitored by analysing Standard Reference Water (OSIL product) alongside all samples. Analytical precision is typically better than 5% variation and accuracy greater than 95%, for a wide range of marine, brackish and freshwater samples.

In addition to the major inorganic nutrients it is also possible to analyse total dissolved organic nitrogen and total dissolved phosphorus using catalytic oxidation chambers prior to detection to convert the samples to phosphate and nitrate respectively. The dissolved organic fractions are then calculated by difference by subtraction of the inorganic fraction from the total fraction. Contact: Tim Brand (E: tim.brand@sams.ac.uk)


High Performance Liquid Chromatography

The HPLC facilities within the Biogeochemistry and Earth Science Department are used exclusively for the measurement of algal photosynthetic pigments in aquatic and sediment samples. The technique uses reversed–phase chromatography (non-polar stationary phase) using either 8 carbon or 18 carbon alkyl bonded silica columns. Also the instrument can be operated in either 'isocratic' mode using a single elutant or 'gradient' mode using two or more elutants that vary in their relative proportions during the course of the analytical cycle. The gradient method of operation allows for clearer separation of fresh and decayed photosynthetic pigments and is normally the preferred method of operation for pigment analysis in sediment samples. Final detection is by spectrophotometric or fluorimeteric methods depending upon the optical properties of the pigment. Calibration of the detectors is performed routinely using natural pigment standards (DHI Water and Environment product). Contact: Tim Brand (E: tim.brand@sams.ac.uk)


Gas Chromatography (trace gas analysis)

SAMS has four gas chromotographs that are used for trace gas analysis:

Two are set up specifically for analysis of volatile sulphur compounds, such as dimethylsulphide. These utilise purge and cryotrap extraction techniques and samples are analysed using a pulse flame photometric detector (PFPD).

The other two systems are set up specifically for headspace analysis of methane using a flame ionisation detector (FID).

All instruments are currently set for analysis of gases at trace concentrations, with detection limits in the low nanomolar concentration range. Gases can be analysed from a range of environmental samples including seawater, freshwater, slurry incubations and biological samples. Contact: Dr Arlene Ditchfield (E; arlene.ditchfield@sams.ac.uk)


Gas Chromatography (analysis of lipids)

The lipids gas chromatography (GC) facility, incorporating GC mass spectrometry, is used for determining and identifying marine lipids in sediment, water and organism samples.

These can be used to determine carbon sources in the marine environment and the feeding habits of selected organisms. In addition, the long carbon chain ketones known as alkenones are also analysed and are used to determine palaeo-sea temperatures in marine sediment cores. 


Total Carbon Analyser (DIC, TA)

The CM250 Automated TC/TIC/TOC Carbon Analyzer is a complete analytical system capable of measuring total carbon, total organic carbon and total inorganic carbon in solid and liquid samples. Using either an automated high-temperature combustion furnace or an automated acidification module and using a highly sensitive coloumetric CO2 detector, the instrument is capable of analyzing carbon in a wide range of marine and environmental samples with high precision.

Contact: Dr Natalie Hicks and Tim Brand (E: tim.brand@sams.ac.uk)


Alpha Counting Detector

We have eight EG&G Ortec 576A dual unit silicon alpha detectors and an EG&G Ortec OCTETE eight port silicon alpha detector giving a total alpha capacity of twenty four alpha detectors each with an energy measuring range of  0-9MeV.

Low level alpha particle detection utilise the electrical characteristics of the semiconductor silicon. Silicon belongs to Group IV of the periodic table and has 4 electrons in its outer shell. These electrons are involved with the bonding of the atoms and require energy to dislodge them from the atom, which can be supplied by nuclear radiation. When a voltage is applied to the semiconductor together with an energy input, such as an alpha particle, the liberated electrons move towards the cathode and the resulting positive 'holes' move towards the anode. Movement of these electrons and holes are recorded produce a small voltage pulse and is recorded as a count. Because alpha particles are readily blocked by other atoms and molecule the detectors each sit in a vacuum cell.

Our facilities are routinely used for measuring naturally occurring uranium 238 series radionuclides but have also been used for the detection of the man-made radionuclides americium, curium and plutonium. Contact: Tim Brand (E: tim.brand@sams.ac.uk)


Gamma Counting Detector

SAMS has three EG&G Ortec High-purity Germanium Coaxial gamma detectors, two Canberra Low Energy Germanium detectors and one Canberra Broad Energy detector.

Germanium detectors are semiconductor diodes having a positive-intrinsic-negative structure (P-I-N) in which the intrinsic region is sensitive to ionising radiation, particularly X rays and gamma rays. As with the mechanism of the alpha detectors, when a voltage is applied together with an energy input such as a gamma photon the charge carrying positive holes and electrons are swept by the electric field to the N and P junctions respectively. This causes a small voltage pulse and is recorded as a count. These detectors must be cooled in order to reduce the thermal generation of the charge carriers and liquid nitrogen at a temperature of 77K is used as the cooling agent.

The SAMS facilities are routinely used for measuring naturally occurring and man-made radionuclides. Contact: Tim Brand (E: tim.brand@sams.ac.uk)


Beta Counting Detector

The Risø low-level beta Geiger-Muller Multicounter system, GM-25-5, uses a steady gas stream of argon (99%) and isobutane (1%) which becomes ionised due to beta particle emission from the sample. The ionised gas particles are collected within a high voltage field, detected as an electric current pulse and recorded as a counting event.

At the SAMS the detector is used exclusively for measuring the activity of the naturally occurring thorium 234 radionuclide. Thorium 234 is widely used as a marine particle tracking radionuclide from which the rates of particle movement within the water column and the upper most depths of marine sediment can be calculated. Contact: Dr Robert Turnewitsch (E: robert.turnewitsch@sams.ac.uk)


Total Organic Carbon Analyzer

The TOC-V (Total Organic Carbon Analyzer) instrument can measure the amount of total carbon (TC), inorganic carbon (IC) and therefore the total organic carbon (TOC) in a sample by oxidative combustion-infrared analysis.  A sample can also be measured simultaneously for the non-purgeable organic carbon (NPOC) and total dissolved nitrogen (TN) in a sample. 

Total nitrogen is measured using the principles of oxidative combustion chemiluminescence. The ASI-V autosampler is used in combination with the main unit allowing automatic analysis of multiple samples. Contact: Sharon McNeill (E: sharon.mcneill@sams.ac.uk)


Automated Nitrogen Carbon Analysis for Gas, Solids and Liquids (ANCA-GSL)

The ANCA-GSL measures not only the total nitrogen or carbon in a sample but also their 15N and 13C levels in a wide range of biological and chemical samples.  The sample is combusted into a gas then passed through a reduction column removing excess oxygen, the gas chromatograph separates the components of interest which pass into the mass spectrometer ionizing the sample and calculating the isotopic levels of carbon and nitrogen. Contact: Sharon McNeill (E: sharon.mcneill@sams.ac.uk).

Seawater trace metal analysis by SeaFAST+ICP-MS

We are GEOTRACES intercalibrated for seawater REE measurements

Introduction

Seawater elements processed by SeaFAST in preconcentration mode (green)The SeaFAST Pico (Elemental Scientific Inc., Nebraska, USA), designed to facilitate seawater trace metal analysis, has been tested by scientists involved in the GEOTRACES programme [e.g. 1, 2], widely recognised as the gold standard of seawater chemical analysis. The SeaFAST is essentially automated column chromatography that allows processing of undiluted seawater for a range of trace metals (Fig. 1 shows seawater elements processed by SeaFAST in preconcentration mode in green).

At SAMS, we have also developed methods to process other samples types, such as digested carbonates and organics, which benefit from preconcentration prior to analysis.


Method and performance

Graph showing comparison of seawater copper signal intensities measured by ICP-MS and SeaFAST+ICP-MSComparison graph of rare earth element concentrationsGraph comparing trace metals in otolithSample uptake into a 10 ml loop and elution of the processed aliquot is controlled by syringe, resulting in highly reproducible column loading and elution. Processing times are typically ~15 mins per sample. Our method for seawater analysis involves indium doping of 24 ml sample volumes to correct for drift, x40 preconcentration by SeaFAST (i.e. double 10 ml loop loading and elution into 0.5 ml), followed by off-line ICP-MS measurement using external standardisation with a 6-point calibration. For higher concentration river or loch waters, a 12 ml sample and single loop loading is used. The combined effects of matrix removal and preconcentration (x200 compared to x10 diluted seawater) greatly increase signal intensity (Fig. 2) and reproducibility (Figs. 3). We have recently achieved excellent reproducibility of trace metal measurements on the certified reference material (CRM) NEIS-22 otolith carbonate standard (Fig. 4).

Our dissolved REE measurements of the BATS (2000 m) seawater have been intercalibrated by the GEOTRACES Standards and Intercalibration Committee (March 2016).


Applications

At SAMS, the SeaFAST is used in a number of projects to measure trace metal concentrations in river water, coastal waters and open ocean water, as well as in other matrices (e.g. coral skeletons, fish otoliths). Current research projects include:

  • >"Iron BREW: Iron Beyond River Etive Water“ – interaction of Fe and DOC in the export of dissolved Fe across salinity gradients in Scottish sea lochs to coastal waters (funded by the MASTS Coastal Processes & Dynamics Forum).
  • >"REEL IT IN: Seawater rare earth elements across the Extended Ellett Line" – sources of rare earth elements to seawater and their water column cycling (funded by a SAMS Small Grant).
  • >"COREE: Groundtruthing rare earth element behaviour in cold water corals" – determination of seawater rare earth element partitioning into aragonite in response to changes in the marine carbonate system (funded by a Research Incentive Grant of the Carnegie Trust).

Although Fe and rare earth elements are the focus of these projects, other elements (V, Mn, Co, Ni, Cu, Zn, U) are routinely measured during sample analysis.


References

[1] Lagerstroem, M. E. et al. Marine Chemistry, 2013. 155: 71-80.
[2] Hathorne, E. C. et al. Geochemistry Geophysics Geosystems, 2012. 13:
[3] van de Flierdt, T. et al. Limnology and Oceanography-Methods, 2012. 10: 234-251.
[4] Wang, B.-S., et al. Talanta, 2014. 128: p. 337-344.
[5] Freslon, N., et al. Geochimica Et Cosmochimica Acta, 2014. 140: p. 177-198.
[6] Taylor, S.R., et al., The Continental Crust: its composition and evolution. 1985, Oxford: Blackwell Scientific Publishers.
[7] Geffen, A.J., et al. Fisheries Research, 2013. 143: p. 67-80.


Contact

Dr Richard Abell (E: richard.abell@sams.ac.uk) for technical enquiries and info@srsl.com for booking information.

Multi-sensor core logging

Our Geotek Ltd multi-sensor core logger (MSCL) is the only commercially available tool for gathering physical property data in an automated, non-destructive and quality-controlled way. The range of parameters that can be measured includes:

  • >p-wave velocity
  • >gamma density
  • >magnetic susceptibility
  • >electrical resistivity
  • >colour imaging
  • >gamma spectroscopy

Typically, the MSCL can log material at rates of 12m h-1 and at sampling intervals of down to 1mm. Its flexibility is such that it can analyse either whole or split (D-section) cores.

Palaeoclimatological applications include: rapid, high resolution visual archives; sediment accumulation rates and chemistry; impedance, permeability and water content profiles; seismic stratigraphy; synthetic seismograms; rapid assessment of core quality; rapid inter core correlations; data rescue from existing core repositories; ice core logging.


Laser particle size analysis

Laser-particle size analysis (PSA) provides detailed information on the sediment grain size distribution and therefore texture.

Textural data can be used to provide an estimate of deposition, transport and erosion rates as well as being a proxy for environmental information such as benthic ecology and biodiversity. We use a Meritics LS230 laser-diffraction Coulter Counter. The technique uses the obscuration of a laser to determine the shape, size and distribution of particles held in suspension. Particle sizes can be measure between 0.004 to 2000 mm (clays to coarse sand). Using this method the distribution of particles within a sediment sample can be studied. Sediment grain size is a reflection of depositional environment and therefore climate. Sediments can either be analysed as bulk wet suspension or pre-treated using acids to remove any organic material that can mask the terrigenous signal.

Contact: Dr John Howe (E: john.howe@sams.ac.uk) for technical enquiries and info@srsl.com for booking information.

Our microbiology capabilities are significant and include the world's most diverse collection of algae and protozoa, numerous microscopes and a number of microbiology related laboratories and temperature-controlled rooms. We also have outstanding expertise in the taxonomic and quantitative analysis of phytoplankton and zooplankton, which can be made available for commercial or government contracts.

Specific equipment includes

  • >Coulter Counter Multisizer 3: mainly used for counting microalgae, it can count cells/particles 0.5-140 um in size and estimate size if particles are relatively sphere shaped. The instrument provides interesting stats such as cells per ml, standard deviation, mean size, cell volume area etc.
  • >Algem Bioreactors: micro- and macroalgae can be grown in 1L vessels under controlled light and temperature conditions. The software includes >80 years global weather data, allowing users to mimic the growth conditions (light intensity, temperature following typical daily patterns) anywhere in the world at all seasons. The bioreactor measures OD, pH, temp, and light intensity. It allows users to calibrate the OD to a cell number for each organism they wish to grow. At SAMS we can grow 6 x 1L vessels at a time with maximum 800ml in each vessel, good for us to triplicate cultures/conditions.
  • >Numerous inverted and standard Zeiss microscopes, some with optional fluorescence illumination and digital image analysis capabilities
  • >Zeiss confocal microscope with Argon laser for the creation of rotating 3D images of cells/microorganisms. It has also the capacity for FRET and FRAP analysis for following dye traced chemicals through a cell over time
  • >EOL 6390LV environmental scanning electron microscope (new in 2007): a low vacuum instrument that can be fitted with an Emitch cool stage for imaging unfixed samples.
  • >JEOL 100S transmission electron microscope with 100kV beam, tungsten filament and photographic plate image capture. A glass knife maker and ultramicrotome are included in the set-up.
  • >Flow cytometery facility (FACSort and FlowCAM)
  • >Cryopreservation facilities
  • >Radiochemistry facility and liquid scintillation counter
  • >Incubators to culture phytoplankton and bacteria
  • >Fermentation and HPLC facilities
  • >Laminar flow hoods, filtration rigs, autoclaves etc

Contact: Elaine Mitchell (E: elaine.mitchell@sams.ac.uk) for technical information and info@srsl.com for booking enquiries. 

Techniques

  • >microbial ecology such as fluorescent in situ hybridisation, denaturing gradient gel electrophoresis and ribosomal RNA gene sequencing
  • >gene cloning and gene expression studies
  • >1-D and 2-D protein electrophoresis
  • >bioinformatics of marine microbial genomes

Equipment

  • >thermal cyclers for PCR and quantitative real-time PCR. 
  • >nanodrop spectrophometer for DNA and RNA quantification
  • >conventional 1- and 2-D gel electrophoresis for RNA, DNA and protein analysis
  • >Agilent 2100 Bioanalyzer, also for RNA, DNA and protein analysis
  • >dedicated electrophoresis room with adjoining dark room equipped with a digital gel capture system or conventional photography (MP4 Landcamera)
  • >fluorescent and colourmetric plate readers for microplate samples 
  • >microcentrifuges and refrigerated benchtop centrifuge that can process up to six 250 ml samples
  • >also fume-cupboard and chemical storage areas

Contact: Dr Mark Hart (E: mark.hart@sams.ac.uk) for technical information and info@srsl.com for booking enquries.