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P R Alves1 and R D Hagni2
ABSTRACT
The carbonatite-hosted apatite deposit at the Cajati open pit mine in the Jacupiranga igneous-carbonatite complex is located in south-eastern Brazil. The major styles of apatite mineralisation include veins or veinlets, small pods or patches, disseminated apatite and locally massive aggregates. The metallurgical concentration of the apatite is accomplished by grinding the carbonatite, removal of magnetite with a magnetic drum, size classification with cyclones and flotation to suppress carbonates and collect apatite. To examine the character of the apatite grains and to apply those observations to apatite beneficiation, specimens of carbonatite were collected from recent exposures in the mine and from selected drill holes. This study utilised a variety of microscopy methods, including transmitted and reflected light, cathodoluminescence (CL) and scanning electron microscopy with wavelength-dispersive spectrometers for mineral compositions. It was found that LREE, Na and Sr are the main elements replacing Ca in the apatite, with relatively low oxide contents (<0.5 per cent, but up to about one per cent for Sr). LREE and Sr contents consistently increase in the latest intrusions (C4, C5 and SP24). Chemical and morphological modifications of apatite were recognised to be related to detrimental effects on flotation recovery. Three examples illustrate this relationship: 1. 2. Apatite with reddish CL is fractured. Locally that apatite exhibits no CL due to CL quenching caused by iron entering the apatite structure. Apatite from the xenolith-rich area exhibits abundant fine, platy silicates that appear to interfere with flotation and lower apatite recovery. So called hard apatite, which is more difficult to grind, occurs in an area in the mine that was affected by hydrothermal activity. That activity is evidenced by the development of a bright, white CL rim in the apatite, and by the presence of late veins of carbonates and sulfides that fill fractures and appear to contribute to higher cohesiveness of those apatite grains.
Jacupiranga, it will be referred to here as the Jacupiranga carbonatite, and the open pit mine that is actively mining phosphate from those carbonatites will be referred as the Cajati mine. The Jacupiranga carbonatite forms an apparently continuous orebody of economic importance with respect to phosphate mining. Despite the fact that the apatite had been known for many years, no previous investigations had emphasised the apatite mineralisation and its association with process mineralogy. The idea for this research project arose from the senior writers daily experience with apatite beneficiation at the mine, together with her scientific interest in investigating the possible correlation of the effect of the character of phosphate ore variations upon the efficiency of the beneficiation process.
3.
INTRODUCTION
Carbonatites are rare rocks that are derived from the Earths mantle. More than 300 known carbonatite localities occur in the world (Kogarko et al, 1995). Due to the growing interest of a small number of researchers, the understanding of the genesis and evolution of carbonatite rocks has significantly increased since the 1960s, when their magmatic origin was experimentally demonstrated by Wyllie and Tuttle (1960). The eruption of very fluid, alkaline carbonatite lava from the Oldoinyo Lengai volcano in Tanzania in 1958 formed a very important milestone in carbonatite understanding (Dawson, 1966). The present study has involved an investigation of the carbonatites from the world-class alkaline igneous-carbonatite complex located at Cajati (formerly a district of Jacupiranga) in south-eastern Brazil. Because the complex is best known as
1. 2. Mineral Scientist, Imerys Pigments, 618 Kaolin Road, Sandersville, Georgia 31082, USA. Email: PaulaAlves@imerys.com Curators Professor of Geology Emeritus, Department of Geological Sciences and Engineering, Missouri University of Science and Technology, 161 McNutt Hall, Rolla MO 65409-0410, USA. Email: rhagni@mst.edu
HISTORY OF THE JACUPIRANGA IGNEOUS COMPLEX (JIC) Discovery and mapping of the complex
The Jacupiranga Igneous Complex was discovered in 1877, and initially the area of carbonatite outcrop was described as an iron ore occurrence because of its high magnetite content. Melcher
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(1954) provided the first detailed mapping and petrographic descriptions of the rocks in the complex, recognised the carbonatites and proposed that they had been intruded during two distinct events. The weathered carbonatites on the top of a smooth hill were already being mined at that time. Continuous development of open pit mining exposed the carbonatite and its host rock clinopyroxenite, providing important exposures for more detailed study. The first geological map of the complex at a scale of 1:25 000 was completed in 1989 by Gaspar, and he subsequently prepared a second map of the mine area at a scale of 1:10 000. Based upon petrological and structural data, he concluded that the carbonatite body was composed of five successive intrusions, a view that is held today. Study conducted by Germann, Marker and Friedrich (1987) served to better outline the contacts of the large dunite body in the northern portion of the complex. The regional geological map of the Jacupiranga Igneous Complex was updated in 1999 on a scale of 1:50 000 and was expanded by the Brazilian geological survey (CPRM) with the purpose of identifying mineral opportunities related to the complex and its country rocks. The main change in the map involved the inclusion of an adjacent satellite body of hornblende-bearing biotite-olivine gabbro that was detected by processing airborne (magnetic and gamma-spectrometric) geophysical data. More detailed mapping of the carbonatites that are well exposed in the mine walls, at a scale of 1:500 for deposit modelling, grade control and other mining-related purposes was initiated in 2000 and has resulted in better delineation of the carbonatite intrusions, marginal dykes and zones of xenoliths.
Approximately 590 000 t of phosphate concentrate was produced at Cajati in 2003, out of a total rock removal of 5 400 000 t/yr of carbonatite plus 6 600 000 t/yr of clinopyroxenite waste. Ore reserve modelling and long-term mine planning have demonstrated that at that rate of production, the estimated remaining open pit mine life will be 17 years. The apatite concentrate is obtained after a process involving grinding, magnetic separation, size classification and finally several stages of flotation. The concentrate is used to produce phosphoric acid, which in turn is applied to manufacture animal feed, fertilisers and food grade phosphoric acid. Igneous apatite is clean and yields concentrates with high P2O5 content. However, as fertiliser, phosphate of igneous origin is released to the soil at a slower rate as compared to phosphate from a sedimentary source. Apatite occurs at Cajati as small, elongated crystals that are generally arranged in continuous, parallel veinlets along the magmatic foliation. Larger crystals usually exhibit prismatic, hexagonal shapes, and they formed at an earlier time in the paragenetic sequence. The average content of apatite in the carbonatites at Cajati is about 12 per cent, which corresponds to five per cent P2O5. The mine cut-off grade is three per cent of P2O5. The average modal concentration of the gangue minerals in the carbonatite phosphate ore is approximately: 54 per cent calcite, 20 per cent dolomite, eight per cent magnetite, two per cent olivine, two per cent phlogopite, one per cent sulfides and less than one per cent of other minerals.
Mining activities
Phosphate mining activities began in 1943, and apatite concentrate has been continuously produced since then. The mine is located at the town of Cajati, which was a district of the town of Jacupiranga in the 1990s. Initially the ore was mined from the weathered rock accumulated on top of the oblate hill called Morro da Mina (Mine Hill). The hill was comprised mainly of the carbonatite body, and it was surrounded by clinopyroxenite (jacupirangite). In the 1960s, phosphate-rich concentrations were also mined in the northern foothill area. It is interesting that recent gravimetric and borehole surveys have confirmed the extension of the carbonatite body into the lowlands north of that hill. The weathered ore was characterised by a high grade (>20 per cent) P2O5, but it was virtually exhausted by the early 1970s. In order to concentrate phosphate from the underlying much lower grade ore (average of five per cent P2O5) in the bedrock, mineral processing based upon flotation was developed. Diverse applications of the resulting tailings have subsequently been developed. Both carbonate and magnetite by-product concentrates are economically useful in the cement industry. The by-product ground carbonate tailings with high magnesium contents are also utilised as soil additives. Part of the fragmented (blasted) clinopyroxenite is further crushed and sold as construction aggregate. Cajati produces apatite from one of the worlds lowest average grade phosphate deposits. With regard to elevations in the open pit, in 2002, phosphate ore was being mined from as low as 70 m below sea level, to as high as 120 m above sea level. The hill originally reached 225 m at its highest topographic level. The Cajati mine was the only relevant source of phosphate in Brazil before the 1970s, when additional carbonatite-related, weathered apatite deposits were developed. By 2003, however, there were four significant phosphate mines in Brazil, and Cajati ranked fourth and represented approximately ten per cent of the national production (DNPM, 2003).
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FIG 1 - Tectonic setting of the Paran Sedimentary Basin, and related main occurrences of alkaline complexes with carbonatites along the margins of that basin (after Gomes, Ruberti and Morbidelli, 1990).
On a more local scale, two tectonic domains can be recognised in the area of Jacupiranga, namely the Ribeira Belt and the Coastal Domain (Vasconcelos et al, 1999). These tectonic units are separated by the Lancinha-Cubatao shear zone, and they are illustrated in Figure 2. The Ribeira Belt, situated north of a shear zone, shows strong NE-SW lineament and comprises a complex association of metavolcanic-sedimentary rocks of low metamorphic grade (with estimated metamorphic peaks dating around 580 Ma and 530 Ma), and it is intruded by large calc-alkaline granite bodies (Vasconcelos et al, 1999). The Ribeira Belt is analogous to the Damara Belt in southern Africa, and both structures represent ancient suture zones of Precambrian amalgamation of microcontinents. The Coastal Domain, south of the Lancinha-Cubatao shear zone, corresponds to a set of supracrustal rocks exhibiting variable degrees of metamorphism, and it forms the Paleoproterozoic basement whose mica-schists and gneisses were later intruded by the Jacupiranga complex (Vasconcelos et al, 1999). Other alkaline-ultramafic igneous complexes are present in the Jacupiranga region, including Juqui, Itapirapun and Mato Preto. They occur as discordant intrusions into rocks of either (or both) tectonic areas, Ribeira Belt and Coastal Domain.
area, in the Ribeira River Valley, can be reached by driving 240 km along the highway BR116, south-west from the city of So Paulo. The Jacupiranga Igneous Complex is an intrusive body that has an outcrop area of about 65 km2 (Ruberti, Gomes and Melcher, 2000). It is an elongated ellipsoid in plan view, the longest dimension of which is oriented in a NNW direction. The complex consists mainly of two ultramafic intrusions: dunites to the north and clinopyroxenites (jacupirangite) to the south. Subordinate amounts of alkaline and other rocks are present in the complex. The carbonatites intrude exclusively into the clinopyroxenite and they outcrop in an area of approximately 0.7 km2. They largely consist of a sequence of pipe-like intrusions with subcircular cross-sections, together with genetically related dykes. Numerous rounded, large xenoliths of the clinopyroxenite (from a few centimetres up to about four or five metres) occur within the carbonatite, especially in the area of the contact between the more magnesium-rich intrusions in the northern portion of the deposit but also within the earlier southern intrusions. Drilling has demonstrated that the carbonatites extend in depth to at least 400 m below sea level, with a plunge of about 80 from the horizontal. Structures in the carbonatites are mainly represented by a fault zone oriented NNW, sets of joints, and fractures. Magma flow structures, such as magmatic foliation are also present. Gaspar (1989, 1991) grouped the rocks of the Jacupiranga complex into three categories:
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FIG 2 - Simplified regional geologic and tectonic domains in the region of the Jacupiranga Igneous Complex (after Vasconcelos et al, 1999).
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FIG 3 - Schematic map of the Jacupiranga Igneous Complex (after Gaspar, 1989; Vasconcelos et al, 1999).
1. 2. 3.
The distribution of those rocks within the complex is given in Figure 3, based on mapping by Gaspar (1989) and on subsequent modifications by Vasconcelos et al (1999).
CATHODOLUMINESCENCE MICROSCOPY
Apatite ore-bearing carbonatite specimens for the present investigation were collected from selected locations in six different areas throughout the open pit Cajati mine (A to F), and from one selected drill hole (SP24) located to the north of the mine area. Those areas are shown on the sampling map (Figure 4), and they correspond approximately to the following intrusions (C1 to C5), as defined by Gaspar (1989): A and B = C1, C = C1 and C2, D = C2 and C3, and E and F = C4 and C5. Carbonatite specimens collected from drill hole SP24 do not correlate with any of Gaspars five intrusions. Most of the specimens selected came from areas C, D, E and F. The specimens were examined by transmitted light petrography, reflected light microscopy and especially by cathodoluminescence microscopy. Mineralogical and textural aspects were carefully described and interpreted for each sample, and a total of 1254 microphotographs were taken to record petrographic observations during the investigation of the thin sections (Alves, 2008). Minerals found to be present in the carbonatites include carbonates (calcite, magnesian calcite, dolomite and rarely strontianite), fluorapatite, magnetite (primary and secondary), ilmenite, olivine (forsterite), phlogopite, sulfides (pyrrhotite,
pyrite, chalcopyrite, valleriite), and minor or secondary phases (baddeleyite, perovskite, goethite, serpentine and the pyrochloregroup). Cathodoluminescence (CL) microscopy is uniquely applicable to the study of many of the minerals present in the Jacupiranga carbonatite. Calcite, dolomite and apatite, which together constitute more than 70 per cent of those rocks, emit distinct CL radiation as visible colours when excited by an electron beam. Carbonatite calcite usually exhibits yellow to yellowish orange CL, and magnesian calcite produces a reddish orange CL. Dolomite typically shows red or brownish red CL. Baddeleyite is present in very small amounts in the Jacupiranga carbonatite but it is readily detected due to its blue CL. Most importantly, as recently emphasised by Waychunas (2002), apatite exhibits a variety of CL colours and can be very effectively studied by cathodoluminescence microscopy. A Technosyn CL instrument mounted on a Nikon microscope, operating with an acceleration voltage from 10 - 15 kV (usually 11 - 12 kV), was used for the present investigation. The CL emission spectrum of a mineral depends largely upon the trace elements present in the mineral, but also upon certain intrinsic properties of some minerals. Apatite from Jacupiranga exhibits several colour shades in the vicinity of blue: light blue, bluish grey, greenish blue, reddish blue, lilac (Figure 5), and it also locally shows white rims. The cause for the CL shown by apatite has previously been shown to be due to the replacement of Ca by minor quantities of Mn and REE (Marshall, 1988). Apatite occurs at Cajati as small, elongated crystals usually arranged in continuous, parallel veinlets along the magmatic foliation. Larger crystals usually exhibit prismatic, hexagonal shapes, and they were formed at an earlier time in the
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FIG 4 - Map showing areas selected for carbonatite specimen collection at the Cajati mine.
paragenetic sequence. The average content of apatite in the carbonatites at Cajati is about 12 per cent. Under the CL microscope Jacupiranga apatite exhibits up to five distinct CL zones (Figure 5). The inner zone of the apatite crystals exhibits a pinkish blue/violet CL. The core of apatite crystals is commonly euhedral, shows a hexagonal shape and may consist of more than one crystal in a cluster. The second zone shows blue CL, and this zone locally can be absent. The third zone shows light blue/ greenish blue CL, a more persistent colour, and it is present in all apatite crystals. The fourth zone has blue CL and is quite similar in CL to zone 2. A fifth zone with bright white CL occurs along the borders of some apatite crystals in the later northern carbonatite intrusions. It is present in those carbonatites that exhibit clear evidence of alteration by local hydrothermal fluids.
FIG 5 - Cathodoluminescence micrograph showing euhedral to subhedral apatite crystals in carbonatite from the Cajati phosphorus mine. The crystals exhibit well-developed growth zoning brought out by distinct variations in the intensity and colour of cathodoluminescence. Specimen J128-C. FOV: 1.5 mm.
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At the beneficiation plant, the first process step is bar milling to further comminute the ore to produce apatite separation from the gangue and to increase the surface area of the particles, a feature that is very important for the flotation step. The bar mills operate in closed circuit with cyclones, so particles larger than 0.5 mm return to the mill. This creates a re-circulating load representing about ten to 20 per cent of the total wet weight inside the mill. The ground ore then undergoes removal of magnetite using wet magnetic drums. The magnetic reject consists mostly of magnetite and ilmenite, but it also contains some apatite inclusions in the magnetite particles that are very difficult to liberate. However, the amount of non-recovered apatite in the magnetic reject is typically very small. After magnetic separation, another set of cyclones is used to deslime (ie remove the fines from the ore slip). Although these fines still contain apatite, they are detrimental to the mechanical flotation cells, and therefore they are subsequently scavenged in air flotation columns. The next process step is flotation to separate apatite from the remaining gangue. Valuable apatite particles are separated from the gangue by their collection on the surface of bubbles. The addition of appropriate chemicals (surfactants and wetting agents) modifies the surface charges of the apatite to be floated, rendering it hydrophobic (ie eliminating its affinity with water). Air is then bubbled through the preconditioned mixture of minerals, water and chemicals. The hydrophobic apatite grains escape the water by attaching to the air bubbles and rising to the surface. The accumulated foam forms a froth containing the concentrated apatite that is then collected. At Cajati, scavenging and cleaning flotation steps are used to increase final apatite recovery. The flotation reject typically contains less than 1.5 per cent of P2O5, but the company would prefer that this content be consistently below one per cent. In order to determine how to further increase recovery, it is required to know and understand the variation of the apatite characteristics throughout the deposit, and the present research has been designed to contribute to that understanding.
Gaspar (1989). The present research has shown that although there are some chemical composition differences that contrast to apatite from the other intrusions at Cajati, the negative effect on flotation recovery probably is mostly a function of the abundant amounts of fine, platy silicates (phlogopite, serpentine) that makes the suppression of these minerals less effective than with apatite ores elsewhere. There is probably an optimum limit for the abundance of platy particles above which they will increasingly make the adhesion of apatite to the bubbles much more difficult. In fact, recent practice by the company has been to limit the mix to less than about 15 per cent weight of mineralised rock from the xenolith zone, although this limiting number may to be somewhat high. A comparison between the economic benefit of ore reserve maximisation versus process recovery maximisation is necessary to determine the break-even point and better define the limit for utilisation of the ore from the xenolith zone.
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For instance, data from the present research has demonstrated important differences in texture and chemical composition between olivine from areas C and E (approximately equivalent to the intrusions C1 and C4, respectively, as delineated by Gaspar, 1989). SEM images from the current research show complex zoning in phlogopite crystals and provide information on the distribution of Ba and Mg between those zones. Both elements are present in highly elevated levels as compared with most carbonatites elsewhere as listed by Brod et al (2001). EPMA of magnetite show variable but low amounts of Ti, Mn, Mg, V and Al, and show the presence of ilmenite laths. The ilmenite contains elevated amounts of Mn, Nb and very high Mg; these results confirm and expand upon the chemical characteristics previously described in the literature by Gaspar and Wyllie (1983a and 1983b). Reflected light microscopic study of the sulfides reveals textures that indicate some of the sulfides are related to hydrothermal activity. Geochemical and mineralogical results from this study also bear upon the Jacupiranga carbonatite genesis. The current study has indicated that more than one petrological process, such as partial melting, fractional crystallisation and hydrothermal alteration, was involved in the development of the individual carbonatite intrusions. The cathodoluminescence petrography is discussed more fully in Alves (2008) and Alves and Hagni (in press).
disseminated, discrete grains; and massive aggregates of medium to coarse apatite grains
developed in the oldest carbonatite intrusion.
Ore characterisation
The apatite from Jacupiranga shows distinctive geochemical trends and textural characteristics between the five carbonatite intrusions. The replacement of Ca was characterised by complex substitutions that occurred under conditions of disequilibrium, simultaneously involving LREE (especially Ce, but also Nd and La), Sr, Na and other less important cations. The total REE oxide level determined for apatite from Jacupiranga in the present research was low, ranging from 0.04 to 0.49 per cent, but with a consistent increase toward the north especially for the three latest intrusions. The content of Na2O also is low and was measured to be between 0.07 and 0.37 per cent in the present research. The variation of LREE levels does not correlate very well with that of Na. In terms of chemical variability among the five intrusions, strontium has the most regular trend, and it also shows a more pronounced sequential increase in the northern intrusions than that shown by LREE. A wider range for SrO content was found (0.40 to 1.02 per cent) than that reported in previous investigations. Strontium typically increases towards the later phases of carbonatite intrusions. Indeed, at Jacupiranga the higher contents of SrO are restricted exclusively to the youngest intrusions in the northern portion of the deposit. Compositional zoning is conspicuous in apatite crystals at Jacupiranga, and it is shown especially by variations in CL colour that are typically the following from core (1) to rim (5): 1. 2. 3. 4. 5. pinkish blue/violet core that commonly shows euhedral hexagonal shapes; blue CL zone that may be absent; light blue/greenish blue zone that is more extensive; blue CL, very similar to zone two; and bright, white CL developed along the borders of some apatite crystals, especially in the northern intrusions that were locally affected by hydrothermal fluids.
The dominant activator for CL in Jacupiranga apatite is Eu+3 (Mariano and Ring, 1975; Roeder et al, 1987). This reflects the typical elevated amounts of the cerium subgroup (LREE) and the relatively low amounts of the quencher element, Fe+2 in the Jacupiranga carbonatites. The interpretation of CL emission spectra from the white zones of apatite at Jacupiranga indicates activation by a broad Mn2+ peak with superimposed peaks for Sm3+, Dy3+ and Tb3+ (Mariano, 2002).
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ACKNOWLEDGEMENTS
Thanks is expressed for financial support to the senior writer (PRA) from the Society of Economic Geologists through a Hugh E McKinstry research grant, and for financial assistance from the Josephine Husbands Radcliffe fund at the Missouri University of Science and Technology. She also thanks colleagues from Bunge Brazil for allowing access to the mine and facilitating the field aspects of this research, and to Maria Cristina Toledo Motta, professor at the Universidade de So Paulo, for first introducing her to the joys of studying carbonatites. She also thanks Robert Pruett at Imerys Pigments for his support during the completion of this research.
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