REVIEW OF SCIENTIFIC INSTRUMENTS

VOLUME 73, NUMBER 7

JULY 2002

The modied Rankine balance: A highly efcient, low-cost method to measure low-temperature magnetic susceptibility in rock samples
A. Hagermanna) and E. Schneppb)
r Geophysik der Westfa lischen Wilhelms Universita t, 48149 Mu nster, Germany Institut fu

Received 19 June 2001; accepted for publication 18 April 2002 In this article, we present a method to measure the relative changes in the magnetic susceptibility of rock samples in the low-temperature range ( 200 C to 20 C. The method differs from other experimental methods currently used in that it requiresin contrast to ac bridges, the most widely used devicesvery little sophisticated laboratory equipment: A high-precision laboratory balance, a Pt-100 thermoelement and a computer with standard input/output interface and analog/digital processing capabilities, as well as a few rare earth magnets, are the only devices needed in addition to standard laboratory equipment. A Dewar container and a few plexiglass panes can either be handcrafted in the workshops of any larger research institute or are commercially available at little cost. The results of our measurements reveal that the temperature-varying magnetic properties of rock samples can be reliably observed. 2002 American Institute of Physics. DOI: 10.1063/1.1487897

I. INTRODUCTION

X T

The magnetic properties of rocks are determined by the content of ferri or antiferromagnetic minerals. The most well-known example is magnetite Fe3 O4 ). For a given mineral, the magnetic properties also depend strongly on the domain state of the mineral grains, which is a function of grain size. While variation of concentration lies in the range of percent, the variation of the mineral type or its domain state can cause variations of several orders of magnitude of the magnetic properties. For many applications of paleomagnetic or rock magnetic measurements, it is desired to have quick measuring procedures in order to characterize the type as well as the domain state of magnetic carriers in a rock. This is possible by observing the change of hysteresis properties with temperature. In the high-temperature range, the el Curie temperature is characteristic for a well known Ne mineral, while in the low-temperature range, the so-called Verwey Morin transition for magnetite hematite reects a change of magnetocrystalline anisotropy at a temperature of 120 K 258 K.1 These transitions can be observed by a change of magnetic susceptibility at low temperatures, but the occurrence is also domain state grain size dependent. Senanayake and McElhinny2 have shown that measuring the temperature dependence of the magnetic susceptibility in the 200 C to 20 C range is a simple method to yield important information about the composition of a rock sample. The quantity observed, dened as X ( T ), represents the ratio of magnetic susceptibility at a given temperature T to the magnetic susceptibility at room temperature (293 K),
a

T . 293 K

Besides temperature dependence, many rock samples also exhibit a dependence of the X ( T ) curve maximum on the frequency of the ac bridge used for the measurement.3 Senanayake and McElhinny2 showed that most basaltic rocks can be assigned into three different groups, depending on their low-temperature characteristics of magnetic susceptibility. With this information, it is possible to assess the suitability of a given sample for certain paleomagnetic measurements.
II. THE METHOD

r Geophysik & Meteorologie, Universita t zu Present address: Institut fu ln, 50923 Cologne, Germany; electronic mail: hagerman@geo.uniKo koeln.de b r Geophysik der Universita t Go ttingen, 37075 Present address: Institut fu ttingen, Germany. Go 0034-6748/2002/73(7)/2655/4/$19.00 2655

Methods to measure the magnetic properties of rock samples at low temperatures usually require high-cost equipment or rather complicated long-term measurements. The experimental devices most widely used are a type of ac hysteresis loop tracer, a modied susceptibility meter MS1, Bartington or an inductivity bridge Kappa bridge, Geofyzika Brno.4,5 Davis6 reverted to the classical method of measuring magnetic properties of materials by means of a balance, a technique that has already been used by Rankine.7 The principle is that a balance measures the magnetic force interacting between a strong magnet placed on the balance and a sample placed close to it. Due to the high precision of modern laboratory balances, Davis obtained a reasonable accuracy for the measurements, using industrial rare-earth magnets.6 One can easily modify the method of Davis and use the Rankine principle to study the low-temperature behavior of the magnetic properties of rock samples. In this case, the precision of the measurement as such, i.e., the absolute force acting upon the magnet, is of little importance. Here, the experiment focuses on the X ( T ) change, and hence, the amplitude of the force signal itself plays only a minor role as a normalizer.
2002 American Institute of Physics

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Rev. Sci. Instrum., Vol. 73, No. 7, July 2002

A. Hagermann and E. Schnepp

FIG. 1. Schematic drawing of the apparatus presented in this article. The rock sample 1 and Pt-100 2 are embedded in plasticine 3 and placed in a Dewar vessel 4. Three plexiglass spacers 5 ensure exact positioning. The Dewar is inserted into a hole in the shroud 6 of the balance and xed using plastic bolts 7, such that there is only a small gap between the Dewar and the actuator magnets 8, connected to the force transducer of the balance 9 by a plexiglass rod 10. To accelerate warming of the sample, compressed air is supplied through a hose 11.

III. EQUIPMENT

The experimental setup is shown in Fig. 1. In our experiments, we made use of a KERN laboratory balance with an absolute accuracy of 0.1 mg. The balance pan was replaced by a plexiglass boom 10 cm in length which was intended to carry three rare-earth magnets cf. Fig. 2. As force actuators, we used three NdFeB industrial magnets with a diameter of 15 mm and a height of 5 mm, available as NeoDeltaMagnets NDM from IBS Magnet Berlin. A eld measurement of a single magnet revealed a magnetic dipole moment of 0.66 Am2 . Placing the magnets on top of each other yields a diameter/height ratio of 1, resulting in an almost ideal magnetic dipole moment of approx. 2 Am2 . High-precision laboratory balances are usually factory equipped with a plexiglass shroud surrounding the balance pan. To support the sample container, a circular hole was cut into the upper plexiglass cover pane and a small Dewar vessel was xed in the hole using three plastic screws. Leaving only a small gap between the magnets and the Dewar, the rock sample can be positioned at 1.5 cm from the top of the actuator magnets. This corresponds to a magnetic eld of about 35 mT at the bottom of the sample. As a consequence of the dipole characteristics of the eld, the bottom part of the sample will dominate the signal most. By turning the sample upside down, inhomogeneities may be identied. Not only the rock samples measured, but also the magnets used as force actuators, exhibit temperature dependent magnetic properties. In the case of the rare-earth magnets used, the manufacturer gives a temperature sensitivity of 0.1%/C, resulting in a substantial decrease of magnetization with temperature. To avoid this effect, the sample has to be thermally insulated from the magnets. Bearing in mind that the eld strength of a dipole eld is a function of distance, the need for a superinsulation like, e.g., a Dewar container, becomes obvious. A household rubberband serves as a gasket between

FIG. 2. Closeup of the plexiglass rod on top of the balance force transducer. On top of the rod, the three NDM rare-earth magnets 15 mm diameter can be seen underneath the Dewar vessel. Inside the Dewar, two of the three plastic spacers can be seen.

the Dewar vessel and the plexiglass cover of the balance, limiting all interactions between the laboratory with its air circulations and the force transducer of the balance to the magnetic interaction of the sample with the actuator magnets. Inside the Dewar vessel 4 cm inner diameter, we glued three plastic spacers to the bottom to allow for a precise positioning of the rock sample. The purpose of these spacers will be explained in the following section.
IV. MEASUREMENT PROCEDURE

After the rock sample, together with a Pt-100, has been covered with plasticine, it is emplaced in the Dewar vessel for a calibration measurement at room temperature. Then, the sample is removed from the container and cooled down to 196 C in liquid nitrogen. The measurement starts when the sample is replaced in the Dewar, with the spacers inside the Dewar ensuring a position identical to that obtained during calibration. After emplacement, the temperature of the sample will gradually approach room temperature, but the warming process can be accelerated by blowing compressed air into the Dewar vessel. Usually, the duration of a single measurement is in the order of 10 to 20 min. A computer is

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Rev. Sci. Instrum., Vol. 73, No. 7, July 2002

Modied Rankine balance

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FIG. 3. Normalized susceptibility vs temperature as recorded with our apparatus. The sample shows a typical group 1 curve. The normalization corresponds to a total force signal of 455 mg.

FIG. 5. Normalized susceptibility vs temperature as recorded with our apparatus top, dotted line, normalized to 58.1 mg and with a susceptibility bridge bottom, solid line. Both measurements show the susceptibility peak at 150 C characteristic of group 3 samples. Note the high resolution of the new method as well as the signal increase after the characteristic peak see Ref. 3.

used to process the X ( T ) signal by recording the balance force as a function of the temperature measured by the thermoelement. After reaching room temperature, the X (20 C) value can serve as a rst indicator of the quality of the measurement. If X ( T 20 C) 1, an error of some kind like displacement of the sample during measurement is likely to have occurred. If X ( T 20 C) 1, the shape of the X ( T ) curve will reveal the magnetic characteristics of the sample, like e.g., the typical magnetite susceptibility peak at 120 K due to the Morin transition.
V. ERROR SOURCES

ture. As the temperature sensor is covered in plasticine together with the rock sample, the Pt-100 temperature is a good indicator of the temperature of the rock sample, but it does not necessarily yield the temperature of the sample itself. Yet, we found this drawback to be of minor relevance during our measurements, the experimental setup as described in this article serving its purpose satisfactorily.

VI. SOME RESULTS

With the calibration of the magnetic force signal yielding an easily examinable quantity, errors due to a movement of the sample inside the container during measurement can easily be isolated by conrming whether X ( T 20 C) 1. It should be noted that, due to the setup of the experiment, a major source of error is the absolute value of the tempera-

FIG. 4. Normalized susceptibility vs temperature as recorded with our apparatus. The sample shows a typical group 2 curve. Total force signal of 87.2 mg.

As we pointed out in the rst section of this article, three different groups of basaltic rocks can be distinguished, as far as their susceptibility is concerned. Group 1 exhibits a monotonic increase in susceptibility from liquid nitrogen to room temperature, group 2 is characterized by a decrease of susceptibility with temperature, and group 3 has a maximum in susceptibility in the range of 170 to 130 C. For a detailed description, refer to Senanayake and McElhinny.2 Among the samples examined in our experiments, we found candidates of each group with the shape of each susceptibility curve closely resembling the ones depicted by Senanayake and McElhinny. We give the results of three basaltic samples taken in the volcanic region of western Germany and Mexico in Figs. 3 through 5. For the samples investigated from Mexico, we could very well reproduce the curve measured with a low-temperature susceptibility bridge Highmore, modied instrument at the paleomagnetic labo noma de Me xico cf. ratory of the Universidad Nacional Auto Fig. 5. Although the presented method is not necessarily better than other methods currently used for examining the magnetic susceptibility of rock samples at low temperatures, its advantages are that it is fast, cheap, and easily usable. However, as the temperature of the susceptibility peak of titanomagnetites decreases with decreasing frequency of the measurement apparatus, a distinction between magnetites and

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Rev. Sci. Instrum., Vol. 73, No. 7, July 2002

1

A. Hagermann and E. Schnepp . O zdemir, Rock Magnetism, Fundamentals and FronD. J. Dunlop and O tiers Cambridge University Press, Cambridge, 1997. 2 W. E. Senanayake and M. W. McElhinny, Phys. Earth Planet. Inter. 26, 47 1981. 3 C. Radhakrishnamurty and S. D. Likhite, Phys. Earth Planet. Inter. 76, 131 1993. 4 S. D. Likhite, C. Radhakrishnamurty, and P. W. Sharabudhe, Rev. Sci. Instrum. 36, 1558 1965. 5 J. Shaw and J. A. Share, Phys. Earth Planet. Inter. 42, 1 1986. 6 R. S. Davis, Meas. Sci. Technol. 4, 14 1993. 7 A. O. Rankine, Proc. Phys. Soc. London 46, 391 1934.

titanomagnetites can not be made using our method. Yet, we can distinguish either of the basalt groups mentioned by Senanayake and McElhinny.2
ACKNOWLEDGMENTS

hnel for The authors would like to thank Dr. Harald Bo valuable comments and suggestions, as well as Frank Bartschat for his assistance with Fig. 2.

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