HIGH-GRADIENT MAGNETIC SEPARATION (HGMS) IN SOIL CLAY MINERAL STUDIES

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1 Clay Minerals (1984) 19, HIGH-GRADIENT MAGNETIC SEPARATION (HGMS) IN SOIL CLAY MINERAL STUDIES J. D. RUSSELL, A. BIRNIE AND A. R. FRASER The Macaulay Institute for Soil Research, Craigiebuekler, Aberdeen AB9 2Q J, Scotland (Received 6 July 1984) ABSTRACT: A modified HGMS system is described in which the inclusion of a peristaltic pump to continuously circulate a suspension of a soil clay through the magnetic trap greatly facilitates the operation of the technique. Application of this purely physical method of mineral separation to a variety of soil clays--using IR spectroscopy to monitor the progress of the separation--illustrates the ease with which magnetic fractions comprising different iron containing clay minerals may be separated from a single soil clay, thereby making these minerals more accessible for further study by other techniques. The conventional technique of magnetic separation of iron-containing minerals is a well known and well tried method which has been used in mineralogy for several decades. In 1979 however, Schultz & Dixon described a modified method--high-gradient magnetic separation (HGMS)--in which clay-size (0.2-2 ~a) particles dispersed at ph in dilute Na2CO 3 solution are passed through a series of tubes containing fine stainless-steel wool held in the field of an electromagnet. At a fixed field of 1.6 Tesla, and under appropriate flow conditions, these authors showed that many iron-containing minerals, including oxides, hydroxides and layer-silicates, could be concentrated on the steel wool. Although the method showed considerable potential, it appears to have been paid little attention, apart from an investigation by Hughes (1982) on iron and aluminium bound to organic matter in tropical soils. This paper describes a modified HGMS method and its application to a selection of soil clays, using infrared (IR) spectroscopy and X-ray diffraction (XRD) to monitor the progress of the fractionation of different iron-containing clay minerals separated at different magnetic field strengths. Apparatus EXPERIMENTAL The apparatus (Fig. 1), based on a 2T electromagnet from a mass spectrograph and a stainless-steel wool magnetic filter, is essentially the same as that described by Schultz & Dixon (1979). To facilitate sample handling and provide more scope for fractionation of iron-containing clay minerals, the apparatus has two modifications: (i) the clay suspensions are continuously stirred and are pumped around the system by a variable-speed peristaltic 9 The Macaulay Institute for Soil Research, 1984

2 772 J. D. Russell et al. FIG. 1. The HGMS apparatus showing the electromagnet (EM), the magnetic filter (MF), the clay suspension reservoir (R), the peristaltic pump (P) and the magnetic stirrer (S). pump; (ii) the magnetic field may be varied by means of a voltage regulator, with an ammeter in the circuit to monitor current. Clays Three clays were selected to illustrate the scope of the HGMS method. They were separated as < 1.4 pm fractions from: (i) the C horizon of a freely drained brown forest soil on Old Red Sandstone (Lower Powburn) of the Laurencekirk Association; (ii) the reddened patches of an outcrop of deeply weathered granite (Bennachie, near Inverurie, Grampian; (iii) the B Fe/Mn horizon of an imperfectly drained brown forest soil with gleyed B and C horizons (Blairmore Estate, Glass, near Huntly, Grampian) of the Strichen Association. The < 1-4 ~ clays were isolated as 0.3% (w/v) aqueous suspensions in distilled water (ph 5.2) for the HGMS procedure. Method Up to 500 ml of clay suspension, ideally not less than 100 ml, is placed in the reservoir and stirred continuously by a magnetic stirring bar. With the electromagnet switched off, the suspension is pumped, by a peristaltic pump, at ~500 ml rain -1 through the system, carefully manipulating the magnetic filter to exclude air bubbles. It was established at this stage that the steel wool in the filter did not physically trap clay. Magnetic fractions of soil clay were separated by running the electromagnet at increasing fields, i.e. current settings, up to the maximum 275 ma. At each current setting the flow

3 HGMS in soil clay mineral studies 773 was continued for 5 min, equivalent to five passes of the original 500 ml through the filter. To collect the trapped fraction the filter was first washed with water, by-passing the reservoir by means of three-way taps, then the power was switched off and the fraction flushed out from the trap with water. Schultz & Dixon (1979) and Hughes (1982) have shown that the method can recover iron minerals quantitatively. Our technique has the more qualitative objective of providing clean, well-separated mineral fractions for further examination. RESULTS Most iron-containing minerals encountered in soil clays are paramagnetic at room temperature or antiferromagnetic, and in a uniform magnetic field would not be expected to experience any relative attraction. In the non-uniform field surrounding the steel wool surfaces, paramagnetic minerals should experience a net attraction to the wool whereas antiferromagnetic minerals, because of equal and opposite nuclear spins, should display no net attraction. Hematite, an example of the latter type of mineral, possesses a small a. %T H Chl Waventl'nber/cm- 1 FIG. 2. IR spectra of KBr pressed disks containing <1.4 /~a clay from Old Red Sandstone. (a) Original clay, (b) 50 ma magnetic fraction, (c) 150 ma magnetic fraction. H hematite; Chl = chlorite.

4 774 J. D. Russell et al. number of crystalline imperfections in which nuclear moments are not parallel, and should therefore behave like a ferrimagnet and show net attraction in a magnetic field. The following examples demonstrate some of these properties for several iron-containing minerals. Lower Powburn clay Several magnetic fractions ranging from 50 ma to 275 ma were separated from the < 1.4 tim clay. They fell into two groups, representative IR spectra of which, together with that of the original sample, are shown in Fig. 2. The spectrum of the original clay shows absorption bands arising from kaolinite/halloysite, illite, chlorite and quartz. The spectrum of the 50 ma fraction, in addition to showing weaker features due to these silicates, exhibits an intense absorption band at 340 cm -1 arising from hematite. Other characteristic hematite bands at 540 and 470 cm -L are overlapped by those of the silicates. In the spectrum of the original clay the 340 cm -1 hematite band is partly overlapped by layer-silicate (kaolinite, illite, chlorite) absorption, but it is clearly very much weaker than that in the 50 ma fraction, indicating a magnetic concentration factor of at least 10, possibly as much as 50. As described above, the hematite is behaving like a weak ferrimagnet and is being preferentially concentrated at a relatively low field, a property with considerable potential to facilitate further study of this phase. In the spectrum of the 150 ma fraction, the 340 cm I hematite band is much weaker than that in the 50 ma fraction, the pattern being dominated by the absorption bands of chlorite. The chlorite thus concentrated must contain structural iron, but the extent to jj1 \ t %T M Wavenund3er/cm FIG. 3. IR spectra of KBr pressed disks containing <1.4 /an clay from weathered granite. (a) Original clay, (b) 200 ma magnetic fraction. M = macaulayite. M

5 HGMS in soil clay mineral studies 775 which the chlorites themselves may be separated by this method was not investigated for this clay. This problem will be discussed later for the Blairmore clay. Small amounts of kaolin minerals and quartz are also present in the 150 ma fraction, and it would appear from the intensity of the band near 825 cm -~ that illite (presumably ferruginous) has also been concentrated in this fraction. The identification of the above minerals from IR spectra was confirmed by XRD. Bennachie clay Another example of an efficient concentration by HGMS of an iron-rich, hematite-like phase is provided by the separation of macaulayite from the fine clay fraction of a deeply weathered granite. From its IR spectrum (Fig. 3) the original clay comprises more than 90% kaolinite and a few percent of illite, the absorption bands of macaulayite only appearing as a new band at about 300 cm -1 and as a slight enhancement at 650 cm-l After only six passes of the original clay suspension through the magnetic filter with the current set at 200 ma, an iron-rich fraction was obtained. Its IR spectrum (Fig. 3) is dominated by the absorption bands of macaulayite, estimated to comprise not less than c I t I B Chl Wavenumber/cm Fro. 4. IR spectra of KBr pressed disks containing < 1.4 #m clay from Blairmore Fe/Mn pan. (a) Original clay, (b) 100 ma magnetic fraction, (c) 275 ma magnetic fraction. L = lepidocrocite; B = biotite; Chl = chlorite.

6 hydrobiotite; 776 J. D. Russell et al. 80% of the fraction. The properties of this new mineral concentrated by the HGMS method have been more fully described by Wilson et al. (1981, 1984). Blairmore clay The clay from the Fe/Mn pan from this imperfectly drained brown forest soil was separated into several magnetic fractions. IR spectra of the original clay and two of the most representative fractions (Fig. 4) showed that the kaolinite which dominates the original clay is only a minor component in the 100 ma fraction, the major mineral in this being lepidocrocite, with characteristic bands at 260, 400 and near 3100 cm -1. Chlorite with enhanced absorption at about 1000 and 470 cm -~ is also present. The spectrum of the 275 ma fraction still shows the presence of lepidocrocite and kaolinite, but the pattern is dominated by absorption bands of chlorite and of a trioctahedral layersilicate. XRD patterns of these magnetic fractions (Fig. 5) confirm the presence of the minerals identified by IR, and clearly indicate that the additional trioctahedral minerals in the 275 ma fraction are biotite and hydrobiotite. The enhanced intensity of the (001) chlorite reflection at 14 A relative to that of the (002) at 7 A in this fraction indicates that the chlorite is probably Mg-rich. In contrast, the chlorite in the 100 ma fraction, for K ~ G 3"1 3"S 4 S b FIG. 5. XRD patterns of oriented aggregates of < 1.4 pm clay from Blairmore Fe/Mn pan. (a) Original clay, (b) 100 ma magnetic fraction, (c) 275 ma magnetic fraction, B = biotite; B/H - Chl = chlorite; G - goethite; H = hornblende; K = kaolinite; L = lepidocrocite; T = talc.

7 HGMS in soil clay mineral studies 777 which the (002) intensity is greater than the (001), is probably more Fe-rich. An alternative explanation for the enhanced intensity of the 14 /~ reflection in the 275 ma trace as arising from the presence of vermiculite can probably be discounted because of the intrinsic narrowness of the peak. Support for the conclusion from XRD, that the chlorites had been fractionated into Fe-rich and more Mg-rich varieties, is obtained from IR spectra of the OH-stretching region after removal of absorbed water from the samples by heating (Fig. 6). The pattern of chlorite OH bands in the 100 ma fraction is broad, consistent with an iron-rich variety (Farmer, 1974). In the spectra of the higher-field fractions, chlorite OH bands are narrower, more clearly resolved and tend to shift to higher wavenumbers are the field increases, characteristics which are consistent with a tendency towards more Mg-enrichment at the expense of iron. This chlorite fractionation is partly responsible for the steady increase in Mg and decrease in Fe from low- to highfield-fractions (Table 1). It is interesting to note from the XRD traces that the iron oxyhydroxides lepidocrocite and geothite are concentrated by at least an order of magnitude in the 100 ma fraction and that hornblende appears uniquely in this fraction. The concentration of these iron-rich minerals in this fraction is reflected in its high iron content measured by electron probe microanalysis (Table 1). a %T B/H Waventet)~/crn- 1 FIG. 6. IR spectra of heated KBr pressed disks containing <1-4 #m clay from Blairmore Fe/Mn pan. (a) Original clay, (b) 100 ma fraction, (c) 125 ma, (d) 150 ma, (e) 275 ma. B/H = biotite/hydrobiotite; Chl = chlorite; K = kaolinite; L = lepidocrocite.

8 778 J. D. Russell et al. TABLE 1. Electron probe microanalyses of clay and HGMS fractions from Fe/Mn pan in poorly-drained brown forest soil, Blalrmore, Scotland. HGMS fractions Original clay ma SiO Al I MgO "3 TiO ' K ' MnO < Fe The content of manganese in the original clay and the magnetic fractions is too small to permit the detection of Mn-minerals by IR or XRD. Table 1, however, clearly shows significant enhancement of Mn in the higher-field fractions, to such effect that vernadite has been positively identified in the magnetic fractions by TEM and electron diffraction (Birnie, unpublished results). CONCLUSIONS 1. The HGMS technique is a rapid, efficient, non-destructive method of separating and concentrating a range of iron-containing minerals including oxides, oxyhydroxides, layersilicates and amphiboles. 2. Manganese minerals can be concentrated suff to permit their identification by electron microscopy. 3. The efficiency of the technique is necessarily mineral-dependent, but is has the potential to concentrate from soil clays trace quantities of unexpected minerals, thereby facilitating their identification by other physical techniques. REFERENCES FARMER V.C. (1974) The Infrared Spectra of Minerals, p Mineralogical Society, London. HUGHES J.C. (1982) High-gradient magnetic separation of some soil clays from Nigeria, Brazil and Colombia. I. The interrelationships of iron and aluminium extracted by acid ammonium oxalate, and carbon. J. Soil Sci. 33, SCHULTZ D.G. & DIXON J.B. (1979) High-gradient magnetic separation of iron oxides and other magnetic minerals from soil clays. Soil Sci. Soc. Am. J. 43, WILSON M.J., RUSSELL J.D., TAIT J.M., CLARK D.R., FRASER A.R. & STEPHEN I. (1981) A swelling hematite/layer-silicate complex in weathered granite. ClayMiner. 16, WILSON M3., RUSSELL J.D., TAIT J.M., CLARK D.R. & FRASER A.R. (1984) Macaulayite, a new mineral from North-East Scotland. Mineral. Mag. 48,

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