doi:10.1016/S0031-9201(03)00063-3
Copyright © 2003 Elsevier Science B.V. All rights reserved.
Inter-laboratory calibration of low-field magnetic and anhysteretic susceptibility measurements
References and further reading may be available for this article. To view references and further reading you must
purchase this article.
Leonardo Sagnotti
,
, a, Pierre Rochetteb, Mike Jacksonc, Fabienne Vadeboinb, Jaume Dinarès-Turella, Aldo Winkler and “Mag-Net” Science Team1a
a Istituto Nazionale di Geofisica e Vulcanologia, Via Vigna Murata 605, 00143, Rome, Italy
b CEREGE, University of Aix-Marseille 3, BP80 13545, Aix en Provence, Cedex 4, France
c Institute for Rock Magnetism, University of Minnesota, Minneapolis, MN 55455, USA
Received 25 October 2002;
revised 27 February 2003;
accepted 2 March 2003. ;
Available online 9 May 2003.
Abstract
Inter-laboratory and absolute calibrations of rock magnetic parameters are fundamental for grounding a rock magnetic database and for semi-quantitative estimates about the magnetic mineral assemblage of a natural sample. Even a dimensionless ratio, such as anhysteretic susceptibility normalized by magnetic susceptibility (Ka/K) may be biased by improper calibration of one or both of the two instruments used to measure Ka and K. In addition, the intensity of the anhysteretic remanent magnetization (ARM) of a given sample depends on the experimental process by which the remanence is imparted. We report an inter-laboratory calibration of these two key parameters, using two sets of artificial reference samples: a paramagnetic rare earth salt, Gd2O3 and a commercial “pozzolanico” cement containing oxidized magnetite with grain size of less than 0.1 μm according to hysteresis properties. Using Gd2O3 the 10 Kappabridges magnetic susceptibility meters (AGICO KLY-2 or KLY-3 models) tested prove to be cross-calibrated to within 1%. On the other hand, Kappabridges provide a low-field susceptibility value that is ca. 6% lower than the tabulated value for Gd2O3, while average high-field susceptibility values measured on a range of instruments are indistinguishable from the tabulated value. Therefore, we suggest that Kappabridge values should be multiplied by 1.06 to achieve absolute calibration. Bartington Instruments magnetic susceptibility meters with MS2B sensors produce values that are 2–13% lower than Kappabridge values, with a strong dependence on sample centering within the sensor. The Ka/K ratio of ca. 11, originally obtained on discrete cement samples with a 2G Enterprises superconducting rock magnetometer and a KLY-2, is consistent with reference parameters for magnetites of grain size <0.1 μm. On the other hand, Ka values from a 2G Enterprises magnetometer and K values from a Bartington Instruments MS2C loop sensor for u-channel and discrete cement samples, will produce average Ka/K values that are unrealistically high if not properly corrected for the nominal volume detected by the sensors for these instruments. Inter-laboratory measurements of K and Ka for standard paleomagnetic plastic cubes filled with cement indicate remarkable differences in the intensity of the newly produced ARMs (with a standard deviation of ca. 21%), that are significantly larger than the differences observed from the calibration of the different magnetometers employed in each laboratory. Differences in the alternating field decay rate are likely the major source of these variations, but cannot account for all the observed variability. With such large variations in experimental conditions, classical interpretation of a “King plot” of Ka versus K would imply significant differences in the determination of grain size of magnetite particles on the same material.
Author Keywords: Rock magnetism; Magnetic susceptibility; Anhysteretic remanent magnetization; Calibration; Instrumentation; Relative paleointensity
Fig. 1. The temperature dependence of low-field magnetic susceptibility (K) for Gd2O3 above 50 K is described by a Curie–Weiss law, χ=C/(T−θ) (with paramagnetic Curie temperature θ=−18 K).
Fig. 2. Rock magnetic characterization of the “pozzolanico” cement. (A) Hysteresis loops indicate that
Ms=0.65 Am
2/kg, with shape and parameters typical of a mixture of mainly SD and some SP (and/or PSD) grains. The grain size equivalent to
Mrs/
Ms (0.31),
Bcr/
Bc (1.91) and
Bcr (50 mT) is about 0.1 μm for magnetite. (B) A thermomagnetic curve (CS-3 attached to a KLY-3 Kappabridge) reveals a rather high Curie point suggesting the dominance of oxidized magnetite. The light (dark) gray curve is the heating (cooling) curve.
Fig. 3. Low-field magnetic susceptibility values obtained on different Gd
2O
3 samples measured on a Kappabridge at the IRM (squares) and CEREGE (circles) laboratories plotted according to sample mass, normalized to the largest sample value. The open circle corresponds to the sample prepared 18 months later (see text).
Fig. 4. Acquisition of an ARM for a cement cubic sample in an AF of 100 mT, as a function of the intensity of the DC bias field. Measurements made at the CEREGE laboratory on a 2G Enterprises in-line system.
Fig. 5. Viscous decay of the ARM for a cement cubic sample. The time refers to the actual time of the day at which the measurement was made.
Fig. 6. ARM acquisition and demagnetization on the cement u-channel in two successive cycles.
Fig. 7. Plot of
Ka (2G Enterprises magnetometer with in-line AF/ARM system) vs.
K (AGICO and Bartington Instruments meters) for the cement samples. Measurements were all done at the INGV laboratory. The ARM was produced using an AF of 100 mT and a DC bias field of 50 μT, both acting along the
Z-axis only.
Ka data were computed from “raw” data, considering the same volume of 8 cm
3 for all measurements. The reference lines reported to estimate concentration and size of magnetite particles (i.e.
King et al., 1982 and
Dunlop and Ozdemir, 1997) are also drawn.
Fig. 8. Illustration of the influence of the AF procedure for ARM acquisition. Measurements were carried out on the same cement u-channel in the same instrument (2G Enterprises superconducting rock magnetometer with in-line AF and ARM capabilities) in the same laboratory (INGV, Rome). The diagram on the left shows the ARM values produced by application of a three-axis AF (
Z,
X and
Y, in sequence) and a constant DC bias field on the
Z-axis only. The diagram on the right shows the ARM values produced by application of an AF and a constant DC bias field on the
Z-axis only. In both cases the peak AF was 100 mT and the constant DC bias field was 50 μT.
Fig. 9. “King plots” of
χa vs.
χ for cubic cement samples as measured in different laboratories (see
Table 4). Circles: susceptibility measurements from the Bartington Instruments MS2 meter; squares: susceptibility measurements from AGICO KLY-2 or KLY-3 Kappabridges. (A) “Original”
χa, with ARM produced at the INGV laboratory (with 100 mT AF applied sequentially along the three orthogonal axes of the samples with a constant DC bias field of 50 μT along the
Z-axis). (B) “New”
χa, as produced at each laboratory (using the same fields).
Fig. 10.
χa vs. AF decay rate:
χa values were normalized to the value obtained with the 2G Enterprises in-line system in the CEREGE laboratory at the highest velocity (30 cm/s, first value in
Table 4). Measurements at variable AF decay rates were obtained in the CEREGE laboratory on the Schonstedt (squares) and 2G Enterprises in-line (triangles) ARM acquisition systems. Circles: data from laboratories other than CEREGE (see
Table 4).
Table 1. List of low-field magnetic susceptibility measurements for standard cubes of Gd2O3

All susceptibility values are in (10−9 m3/kg) and are corrected to 20 °C. For the KLY-2 Kappabridge, both the standard (4 cm internal diameter) and the large (8 cm internal diameter) pick-up coils were employed.
Table 2. Gd2O3 magnetic susceptibility values, corrected to 20 °C, from different laboratories

Measurements from the MS2B sensor are reported for the low frequency field. Bold values are the mean of 10 samples; Fd% is the frequency dependence of low-field magnetic susceptibility; Diff% is percentage difference normalized to the mean INGV KLY-2 value (1743.1).
Table 3. High-field measurements on Gd2O3 samples from the IRM, Grenoble and CEREGE laboratories

Corrected values for the MPMS are based on an empirical calibration curve derived from measurements of homogeneous solid ceramic cylinders of 5 mm diameter and varying lengths.
Table 4. ARM, χa and χ measurements on cement cubic samples, from different laboratories

Original ARM values are normalized to the value measured at the INGV laboratory before distribution between laboratories. The AF decay rate refers to the ARM acquisition procedure.
Corresponding author. Tel.: +39-0651860321; fax: +39-0651860397.
1 Barbara Maher, Eva Moreno: University of Lancaster, UK; Monika Hanesch, Robert Scholger: University of Leoben, Austria; Robert Jude, John Shaw: University of Liverpool, UK; Gregg McIntosh, Maria Luisa Osete: University of Madrid, Spain; Jürgen Matzka, Nikolai Petersen: Ludwig-Maximilians-Universität München, Germany; Juan Cruz Larrasoaña, Matthew O’Reagan, Andrew P. Roberts: University of Southampton, UK; Tom Mullender, Clare Peters: University of Utrecht, The Netherlands; Kais J. Mohamed, Daniel Rey: University of Vigo, Spain; Jacqueline Hannam, Friedrich Heller: Institut für Geophysik, ETH Zürich, Switzerland; Thomas Frederichs, Ulrich Bleil: University of Bremen, Germany.