ICP Solution laboratory

Lady working in the lab

ICP Solution laboratory Laboratory performs quantitative or semi-quantitative analysis to determine the elemental concentrations in natural and industrial materials. For this the laboratory uses inductively coupled plasma (ICP) mass spectrometry (MS) and optical emission spectroscopy (OES). The protocols for digestion and sample preparation allow to determine most major, minor and trace elements between Li and U.

With emphasis on geoscience, analyses are routinely carried out on various solid or liquid state materials. Our laboratory routines are developed with the main purpose to analyse natural occurring materials including industrial worked compounds and alloys based on natural materials. This includes for instance:

  • rocks and minerals
  • carbonates and phosphates
  • soil and combustion products (e.g. fly-ashes)
  • natural (and waste) waters and saline brines
  • biogenic materials such as otoliths, teeth, bones, horn, shells, eye lenses and akin
  • manufactured materials from industry and science like ore products, solar panels, REE- and Li-containing materials, concrete and alike

Based on a continuous focus on research and development of our laboratory methods, we can offer a unique high-quality expertise within the fields of earth and material science, bio-geoscience, and associated fields where elemental (or isotopic) analysis of natural and natural-based industrial materials are important.

Analyses performed at the facility

The laboratory offers quantitative and semi-quantitative analyses. Custom methods including additional analytical requirements can be setup and performed on request. We are always open to discuss how to assist and to develop new or improve on our analytical approaches. The list of methods below is carried out on a routine basis.

  • Full package: Highly accurate determination of the abundance of 46 major, minor and trace elements by combined ICP-OES and ICP-MS analysis. This method is often the preferred approach for many rock, soil, and mineral samples. Major elements: Si, Al, Ca, K, Na, Mg, Mn, Fe, P, Ti (usually measured by ICP-OES). Trace elements: Li, Sc, V, Cr, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, Pb, Th, U (usually measured by ICP-MS).

  • Quantitative trace element analysis is a robust ICP-MS quantification method to acquire highly precise and accurate elemental concentrations of usually the 41 elements; Li, Mg, Al, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, Pb, Th, U. It is often used on rock, soil or mineral samples where only trace elements are required, e.g. where major element abundances were already measured. 

  • Arsenic (As) analysis is a special quantitative ICP-OES method used on water samples for environmental purposes. It includes the elements Ca, Al, Si, P, Fe, Mg, Mn, Mg, Cu and As.

  • TotalQuant: Semi-quantitative method including the 71 elements; Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Cl, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Rb, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, Zr. It is typically used for screening purposes, e.g. to 'fingerprint' the chemistry of samples prior to a more robust element quantification and is regularly used on water samples.

  • Isotopic analysis is a newly added option using our ICP-MS that can determine the abundance of e.g. Li isotopes (6Li and 7Li) from Li-battery or Li-ore materials.

Sample Preparation Laboratory

Normally the solution analyses require 5 to 10 ml of sample material. For solid samples, usually 5-10 grams of fine grained (i.e. with a homogenised grain size of < 100 µm) material is sufficient. We do not have special demands regarding the packaging used for the storage of the materials to be analysed other than they do not leak or can be contaminated.

Together with our well-equipped Sample Preparation Laboratory we are usually able to take care of any necessary sample preparation step from the raw material state to an analytically ready product. If required, we can perform all the material defragmentation and fine crushing, grinding, dissolution and digestion, or any other kind of sample preparation prior to the solution of the material and the ICP analysis.

Quality control (QA/QC) of the analyses

Performance tests are one of the most efficient ways for an analytical laboratory to monitor the quality of the analyses being performed. Since the installation of our first ICP-MS in 1999, the laboratory has participated in IAG's proficiency test program (GeoPT), where we continuously produce robust accurate and precise results. Approximately 110 analytical laboratories from around the world contribute to this proficiency test program. The biannual performance tests of the GeoPT program are designed to be an external quality control performed on a regular basis for the analysis of a wide range of natural geological materials.

Purpose and Key Instruments and associated facilities

The ICP facility includes a Nexion 1000 quadrupole ICP-MS and an Avio 500 ICP-OES, both from PerkinElmer, that has been operational since 2022. The AVIO 500 is a fully simultaneous ICP-OES instrument equipped with dual view. The UV detector operates with an extended ultraviolet wavelength range from 165 to 403 nm, and the VIS detector covers the visible wavelength range from 404 to 782 nm. The patented Flat Plate™ plasma technology delivers a robust plasma with reduced maintenance. The Nexion 1000 instrument has a high-throughput system equipped with a triple cone interface and quadruple ion deflector. The setup allows to control the ion beam thus increasing accuracy and efficiency. Furthermore, the instrument has a dual mode detector enabling to increase counting data. 

Lady working in the lab Laboratory instruments

Key instrument capabilities:

  • Quantitative analyses of most elements in the range from 6Li to 238 U.
  • Determination of most elements at ppm to ppb level as well as percent level for major elements. 
  • Lower detection limits at ppb to low ppm level.
  • Pt cones are used routinely.
  • For calibration of the instruments certified solutions containing REE and additional elements are employed.

Autosamplers from Teledyne Cetac (models ASX-280 and ASX-560) are connected to the instruments.

  • to offer researchers, companies, consultants, students and organisations chemical and isotopic analyses applicable to science projects and for industrial purposes.
  • to contribute to scientific and applied research through the production of robust and high-quality chemical analyses
  • to offer our analytical expertise tailored to the natural sciences.
  • to improve existing and develop new methods for the application of ICP-MS and ICP-OES analysis to be able to assist at the highest level in scientific and applied research.

In addition to our facilities in the Sample Preparation Laboratory we have equipment to perform the sample preparation procedures listed below.

  • Dissolution by hydrofluoric (HF) acid is a routine procedure in the laboratory to dissolve solid inorganic materials prior to analysis. The samples are fully digested using nitric acid (HNO3) and hydrofluoric acid (HF). The digestion is performed using sample preparation blocks (SPB) from a Savillex HPX-100. The SPB digestion blocks introduce less contamination, has a high sample throughput, and provide a steady temperature for a reliable and reproducible operation. The sample preparation uses 0.1000 g of sample material weighed directly into a PTFE digestion vessel, and 1 mL HNO3, 5 mL HF is added. The samples are then heated in the SPB at 130 °C for at least 48 hours, then fully evaporated at 100° C. Nitric acid is now added and the sample is evaporated once more, in total two times. Nitric acid, an internal standard solution (Ge, Rh, Re) and deionised water is then added, the vessel is closed and placed on the SPB at 130 °C for at least 12 hours. The sample is then diluted in vials with deionized water to 50 ml.

Woman working in the lab

  • Borate melting is a preparation approach that produces borate discs (fused bead) from the sample material, and are used analysing Si abundance, and to fully dissolve difficult samples with e.g. Zr and Hf prior to trace element ICP-MS analysis of zircon, chromite, or similar minerals. An amount of 0.1 g of finely crushed sample is mixed with 0.9 g of sodium tetraborate and fluxed for 30 minutes in a Pt/Au crucible on a rotary table. The resulting fused glass bead is treated with diluted nitric acid in a PP tube digestion vessel placed on a shake table and mixed until the glass bead is fully dissolved in acid. For verification we bracket our analyses using international reference samples like BHVO-2, BCR-2, OU-6, OShBo, and an inhouse basalt standard Disko-1, as well as Gonv-1 (GeoPT-45 standard), BVA-1 (GeoPT -49 standard) can be prepared using the same methods as for the samples.

Woman working in the lab

  • Loss on ignition: If the samples include a large proportion of organic material, the laboratory offers the possibility to measure the loss of ignition prior to the determination of element concentrations analysis.

Current and former project collaborators

  • University of Copenhagen, Dept. of Geosciences and Natural Resource Management (IGN) and Department of Biology
  • DTU Aqua
  • Natural History Museum of Denmark
  • National Museum of Denmark
  • Aarhus University, Department of Geoscience
  • Museum Nordsjælland
  • Industry with focus on waste water and material science.

The publications listed below are an incomplete record of examples where the ICP-MS Laboratory has contributed with analyses and reporting on collaborative projects.

 Scientific articles:

  • Storey, M., Pedersen, A. K., Stecher, O., Bernstein, S., Larsen, H. C., Larsen, L. M., Baker, J. & Duncan, R. A. 2004. Long-lived postbreakup magmatism along the East Greenland margin: Evidence for shallow-mantle metasomatism by the Iceland plume. Geology 32, 173-176.
  • Brandt FE, Holm PM, Søager N (2017) South to north pyroxenite-peridotite source variation correlated with an OIB to arc type enrichment of magmas from the Payenia backarc of the Andean Southern Volcanic Zone (SVZ). Contributions to Mineralogy and Petrology.
  • Holm PM, Søager N, Alfastsen M & Bertotto, GW (2016) Subduction zone mantle enrichment by fluids and Zr-depleted crustal melts as indicated by backarc basalts of the Southern Volcanic Zone, Argentina. Lithos 262, 135-152
  • Larsen, L.M., Pedersen, A.K., Tegner, C., Duncan, R.A., Hald, N. & Larsen, J.G. 2016. Age of Tertiary volcanic rocks on the West Greenland continental margin: volcanic evolution and event correlation to other parts of the North Atlantic Igneous Province. Geological Magazine 153 (3), 487?511. DOI: 10.1017/S0016756815000515.
  • Søager N, Portnyagin M, Hoernle K, Holm PM, Hauff F, Garbe-Schönberg D (2015) Olivine major and trace element compositions in southern Payénia basalts, Argentina: evidence for pyroxenite-peridotite melt mixing in a backarc setting. Journal of Petrology 56, 1456-1494.
  • Thórarinsson SB, Söderlund U, Døssing A, Holm PM, Ernst RE & Tegner C (2015) Rift magmatism on 1 the Eurasia basin margin: U?Pb baddeleyite ages of alkaline dyke swarms in North Greenland. Journal of the Geological Society of London. DOI:10.1144/jgs2015-049.
  • Søager N, Holm PM & Thirlwall MF (2015) Sr, Nd, Pb and Hf isotopic constraints on mantle sources and crustal contaminants in the Payenia volcanic province, Argentina. Lithos 212-215, 368-378.
  • Holm, P.M., Søager, N., Dyhr, C.T., Nielsen, M.R. (2014) Enrichments of the mantle sources beneath the Southern Volcanic Zone (Andes) by fluids and melts derived from abraded upper continental crust. Contributions to Mineralogy and Petrology. DOI: 10,1007/s00410-014-1004-8.
  • Larsen, L.M., Pedersen, A.K., Tegner, C. & Duncan, R.A. 2014. Eocene to Miocene igneous activity in NE Greenland: northward younging of magmatism along the East Greenland margin. Journal of the Geological Society, London 171, 539?553.
  • Søager, N. Holm, P.M. (2013) Melt-peridotite reactions in upwelling EM1-type eclogite bodies: constraints from alkaline basalts in Payenia, Argentina. Chemical Geology 360-361, 204-219.
  • Dyhr, C.T., Holm, P.M., Llambías, E.J. (2013) Geochemical constraints on the relationship between the Miocene-Pliocene volcanism and tectonics in the Mendoza Region, Argentina; new insights from 40Ar/39Ar dating, Sr-Nd-Pb isotopes and trace elements. Journal of Volcanology and Geothermal Research 266, 50-68.
  • Dyhr, C.T, Holm, P.M., Llambías, E. J., Scherstén, A. (2013) Subduction controls on Miocene back-arc lavas from Sierra de Huantraico and La Matancilla, Argentina and new 40Ar/39Ar dating from the Mendoza Region. Lithos 179, 67-83.
  • Søager, N., Holm, P.M., Llambías, E.J. (2013) Payenia volcanic province, southern Mendoza, Argentina: A plume generated back-arc province? Chemical Geology 349-350, 36-53.
  • Larsen, L.M., Pedersen, A.K., Sørensen, E.V., Watt, W.S. & Duncan, R.A. 2013. Stratigraphy and age of the Eocene Igtertivâ Formation basalts, alkaline pebbles and sediments of the Kap Dalton Group in the graben at Kap Dalton, East Greenland. Bulletin of the Geological Society of Denmark 61, 1-18.
  • Thorarinsson SB, Holm PM, Huggler AaJ, Duprat HI, Tegner C (2012) Petrology and geochemistry of the Late Cretaceous continental ignimbrites, Kap Washington peninsula, North Greenland. Journal of Volcanology and Geothermal Research 219, 63-86.
  • Thorarinsson SB, Holm PM, Duprat, H, Tegner C (2011): Silicic magmatism associated with Late Cretaceousrifting in the Arctic Basin ? petrogenesis of the Kap Kane sequence, the Kap Washington Group volcanics, North Greenland. Lithos 125, 65-85.
  • Søager N, Holm PM (2011) Changing compositions in the Iceland plume; Isotopic and elemental constraints from the Paleogene Faroe flood basalts. Chemical Geology 280, 297-313.
  • Holm PM, Pedersen LE, Højsteen (2010) Geochemistry and petrology of mafic Proterozoic and Permian dykes on Bornholm, Denmark: Four episodes of magmatism on the margin of the Baltic Shield. Bulletin of the Geological Society of Denmark 58, 35-65.
  • Dyhr CT, Holm PM (2010) A volcanological and geochemical investigation of Boa Vista, Cape Verde Islands; 40Ar/39Ar geochronology and field constraints. Journal of Volcanology and Geothermal Research 189, 19-32.
  • Søager N & Holm PM (2009) Extended correlation of Paleogene Faroe Island and East Greenland plateau basalts. Lithos 107, 205-215.
  • Larsen, L.M. & Pedersen, A.K. 2009. Petrology of the Paleocene picrites and flood basalts on Disko and Nuussuaq, West Greenland. Journal of Petrology 50, 1667-1711.
  • Larsen, L.M., Heaman, L.M., Creaser, R.A., Duncan, A.R., Frei, R. & Hutchison, M. 2009. Tectonomagmatic events during stretching and basin formation in the Labrador Sea and the Davis Strait: evidence from age and composition of Mesozoic to Palaeogene dyke swarms in West Greenland. Journal of the Geological Society, London 166, 999?1012.
  • Holm PM, Grandvuinet T, Wilson JR, Friis J, Plesner S & Barker AK (2008) An 40 Ar- 39 Ar study of the Cape Verde hot spot: Temporal evolution in a semistationary plate environment. Journal of Geophysical Research, 113, B08201. DOI:10.1029/2007JB005339.
  • Duprat HI, Friis J, Holm PM, Grandvuinet T & Sørensen RV (2007) The volcanic and geochemical development of São Nicolau, Cape Verde Islands: Constraints from field and 40Ar/39Ar evidence. Journal of Volcanology and Geothermal Research 162, 1-19.
  • Holm PM, Wilson JR, Christensen BP, Hansen L, Hansen SL, Hein KM, Mortensen AK, Pedersen R, Plesner S & Runge M (2006) Sampling the Cape Verde Mantle Plume: Evolution of Melt Compositions on Santo Antão, Cape Verde Islands. Journal of Petrology 47, 145-189.
  • Pedersen, A. K. & Larsen, L. M. 2006. The Ilugissoq graphite andesite volcano, central Nuussuaq, West Greenland. Lithos 92, 1-19.
  • Dalhoff, F., Larsen, L.M., Ineson, J., Stouge, S., Bojesen-Koefoed, J. Lassen, S., Kuijpers, J., Rasmussen, J.A. and Nøhr-Hansen, H. 2006. Continental crust in the Davis Strait: new evidence from seabed sampling. Geological Survey of Denmark and Greenland Bulletin 10, 33?36.
  • Schovsbo, N.H., 2003. Geochemical composition and provenance of Lower Palaeozoic shales deposited at the margins of Baltica. Bulletin of the Geological Society of Denmark 50, 11?27.
  • Larsen, L. M., Pedersen, A. K., Sundvoll, B. & Frei, R. 2003. Alkali picrites formed by melting of old metasomatised lithospheric mantle: Manîtdlat Member, Paleocene of West Greenland. Journal of Petrology 44, 3?38.
  • Larsen, L. M., Fitton, J. G. & Pedersen, A. K. 2003. Palaeogene volcanic ash layers in the Danish Basin: compositions and source areas in the North Atlantic Igneous Province. Lithos 71, 47?80.
  • Surlyk, F., Stemmerik, L., Ahlborn, M., Harlou, R., Lauridsen, B.W., Rasmussen, S.L., Schovsbo, N., Sheldon, E., Thibault, N., 2010. The cyclic Rørdal Member ? a new lithostratigraphic unit of chronostratigraphic and palaeoclimatic importance in the upper Maastrichtian of Denmark. Geological Society of Denmark Bulletin 58, 89?98.
  • Barker AK, Holm PM, Peate DW, Baker JA (2009) Geochemical stratigraphy of submarine lavas (3-5 Ma) from the Flamengos Valley, Santiago, Cape Verde. Journal of Petrology 50, 169-193.
  • Holm PM & Prægel N-O (2006) Cumulates from primitive rifting-related East Greeenland Paeleogene Magmas: the Ultramafic Complexes at Kælvegletscher and near Kærven. Lithos 92, 251-275
  • Prægel NO & Holm PM (2006) Lithospheric origin of high-MgO basanites from the Cumbre Vieja volcano, La Palma, Canary Islands and evidence for temporal variation in plume-source influence. Journal of Volcanology and Geothermal Research 149, 213-239.
  • Jørgensen JØ & Holm P M (2002) Temporal source variation and carbonatite contamination in primitive ocean island volcanics from Sao Vicente, Cape Verde Islands. Chemical Geology, 192, 249-267.

Scientific articles:

  • Postma, D.; Pham, T. K. H.; Sø, H. U.; Hoang, V. H.; Vi, M. L.; Nguyen, T. T.; Larsen, F.; Pham, H. V.; Jakobsen, R. A Model for the Evolution in Water Chemistry of an Arsenic Contaminated Aquifer over the Last 6000 Years, Red River Floodplain, Vietnam. Geochim. Cosmochim. Acta 2016, 195, 277-292.
  • Nguyen, T. H. M.; Postma, D.; Pham, T. K. T.; Jessen, S.; Pham, H. V.; Larsen, F. Adsorption and desorption of arsenic to aquifer sediment on the Red-River floodplain at Nam Du, Vietnam. Geochim. Cosmochim. Acta 2014, 142, 587?600.
  • Postma, D.; Larsen, F.; Thai, N. T.; Trang, P. T. K.; Jakobsen, R.; Nhan, P. Q.; Long, T. V.; Viet, P. H.; Murray, A. S. Groundwater Arsenic Concentrations in Vietnam Controlled by Sediment Age. Nat. Geosci. 2012, 5 (9), 656?661.

Scientific articles:

  • Hovmand MF, Rønn R, Kystol J (2017, in press) Energy wood combusted at two Danish Power Plants and evaluation of element concentrations in wood ash. Elsevier, Biomass and Bioenergy
  • Qin J, Hovmand MF, Ekelund F, Rønn R, Christensen S, Groot GAd, Mortensen LH, Skov S, Krogh PH (in press) Wood ash application increases pH but does not harm the soil mesofauna. Environmental Pollution.
  • Cruz Paredes C, Lopez Garcia A, Rubæk GH, Hovmand MF, Sørensen P & Kjøller R (2017) Risk assessment of replacing conventional P fertilizers with biomass ash: residual effects on plant yield, nutrition, cadmium accumulation and mycorrhizal status. Science of the Total Environment, 575, 1168-1176. DOI: 10.1016/j.scitotenv.2016.09.194
  • Hovmand MF, Kystol J, (2013) Atmospheric element deposition in southern Scandinavia Atmospheric Environment 77, 482-489.
  • Hovmand MF, Nielsen SP, Johnsen I (2009) Root uptake of lead by Norway spruce grown on 210Pb spiked soils. Environmental Pollution 157, 404-409
  • Hovmand MF, Kemp K, Kystol J, Johnsen I, Riis-Nielsen T, Pacyna JM (2008) Atmospheric heavy metal deposition accumulated in rural forest soils of southern Scandinavia. Environmental Pollution 1-5.

Reports and Popular articles:

  • Mads F. Hovmand & Jørgen Kystol, (2011). Det regner med sølv. Atmosfærisk nedfald af tungmetaller over København. KTC, Teknik & Miljø, Nr. 2
  • Hovmand MF (2010). Atmosfærisk deposition af tungmetaller og andre sporelementer i Storkøbenhavn. Omfatter målinger fra perioden 1908-2009. Rapport til Københavns Kommune Teknik og Miljøforvaltning
  • Hovmand MF (2008). Atmosfærisk deposition af tungmetaller og andre sporelementer i Storkøbenhavn. Rapport til Københavns Kommune Teknik og Miljøforvaltning. Dec. 2008.

Scientific articles:

  • Nielsen NH, Kristiansen SM (2013) Identifying ancient manuring: traditional phosphate vs. multi-element analysis of archaeological soil. Journal of Archaeological Science, 42, 390-398. DOI: 10.1016/j.jas.2013.11.013.
Tonny Bernt Thomsen
Senior Researcher
Mapping and Mineral Resources
Phone+45 91333885
Publications
Olga Nielsen
Bachelor of Engineering
Mapping and Mineral Resources
Phone+45 91333874
Karina Ditte Stausholm
Laboratory Technician
Mapping and Mineral Resources
Phone+45 91333776

Prices and access to the laboratory

Please contact the Chief technician or Laboratory manager for further information.

The work in the laboratory includes strong acids (hydrofluorid acid, hydrochloric acid, nitric acid) following standardized protocols, which is carried out by our experienced laboratory staff. Thus, for safety-related reasons, we allow only restricted access to the facilities and according to arrangement with the laboratory staff members.

Location

Mapping and Mineral Resources rooms 2-333, 2-335, 2-339.

Sample Preparation Laboratory