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W O R K S H O P Indicator mineral methods in mineral exploration Indicator mineral methods in mineral exploration Workshop 21 August 2011 25th International Applied Geochemistry Symposium 2011 22-26 August 2011 Rovaniemi, Finland Beth McClenaghan, Vesa Peuraniemi and Marja Lehtonen Publisher: Vuorimiesyhdistys - Finnish Association of Mining and Metallurgical Engineers, Serie B, Nro B92-4, Rovaniemi 2011 McClenaghan, B., Peuraniemi, V. and Lehtonen, M. 2011. Indicator mineral methods in mineral explora- tion. Workshop in the 25th International Applied Geochemistry Symposium 2011, 22-26 August 2011 Ro- vaniemi, Finland. Vuorimiesyhdistys, B92-4, 72 pages. Cover – Irma Varrio Content – Elizabeth Ambrose ISBN 978-952-9618-70-5 (Printed) ISBN 978-952-9618-71-2 (Pdf) ISSN 0783-1331 © Vuorimiesyhdistys This volume is available from: Vuorimiesyhdistys ry. Kaskilaaksontie 3 D 108 02360 ESPOO Electronic version: http://www.iags2011.fi or http://www.vuorimiesyhdistys.fi/julkaisut.php Printed in: Painatuskeskus Finland Oy, Rovaniemi Indicator mineral methods in mineral exploration Beth McClengahan1, Vesa Peuraniemi2 and Marja Lehtonen3 1 Geological Survey of Canada, E-mail: bmcclena@nrcan.gc.ca 2 University of Oulu, E-mail: vesa.peuraniemi@oulu.fi 3 Geological Survey of Finland, E-mail: marja.lehtonen@gtk.fi Abstract This one-day workshop builds on the success of the indicator mineral workshop held at the 25th International Applied Geochemistry Symposium. This workshop will review principles, methods, and developments in the application of indicator mineral methods to mineral exploration. In the 1970s and 1980s, indicator mineral methods were used mainly for tin and tungsten and gold prospecting. Since playing a key role in the discovery of the Lac de Gras diamond field in northern Canada in the 1990s, indicator mineral methods have risen in prominence. The scope of the method has expanded, and the range of commodities being sought has broadened to include base and rare metals, as well as diamond and precious metals. The workshop consists of presentations by some of the most experienced practitioners in the field. Indicator mineral methods applied to exploration for gold, porphyry Cu, rare metals, magmatic Ni-Cu and diamonds will be presented as well as heavy mineral recovery methods, the application of Fe oxide mineral chemistry, and the value of sulphides and sulphate minerals. Workshop 3 Program Sunday, 21 August 2011, Hotel Santa Claus, Rovaniemi 8:30 - 8:45 am Registration 8:45 - 9:00 am Introduction Beth McClenaghan and Vesa Peuraniemi (Conveners) 9:00 - 9:30 am Sample processing methods for recovery of indicator minerals from surficial sediments, Beth McClenaghan, Geological Survey of Canada, Canada 9:30 - 10:00 am Indicator minerals in diamond exploration: a case study from eastern Finnmark, Arkhangelsk and the Devonian Belt (Estonia, Lithuania, Novgorod and Pskov), Pavel Kepezhinskas, Kimberlitt AS, Norway 10:00 - 10:30 am Exploring for RE and REE mineralization using indicator minerals Marja Lehtonen, Geological Survey of Finland, Finland 10:30 - 10:45 am COFFEE BREAK 10:45 - 11:15 am Placer gold microchemistry in conjunction with mineralogy and mineral chemistry of heavy mineral concentrates to characterise bedrock sources Norman Moles, University of Brighton, UK 11:15 - 11:45 pm Applicability of sulphide and sulphate minerals in heavy mineral studies, Vesa Peuraniemi, University of Oulu, Finland 11:45 - 1:00 pm LUNCH 1:00 - 1:30 pm Application of iron-oxide discriminant plots in mineral exploration, Georges Beaudoin, Université Laval, Canada 1:30 - 2:00 pm Porphyry Cu indicator minerals in glacial till samples around the giant Pebble Porphyry Cu-Au-Mo deposit, Alaska, Bob Eppinger, US Geological Survey, USA 2:00 - 2:30 pm Heavy mineral assemblages in Devonian sandstones and Quaternary sediments in Latvia, Vija Hodireva, University of Latvia, Latvia 2:30 - 2:45 pm COFFEE BREAK 2:45 - 3:15 pm Kimberlite indicator mineral based diamond exploration programmes in Karelia, North-West Russia, Vladimir Ushkov, Karelian Geological Expedition, Russia 3:15 - 3:45 pm Till indicator mineral and geochemical signatures of magmatic Ni-Cu deposits, Thompson Nickel Belt, central Canada, Beth McClenaghan, Geological Survey of Canada 3:45 - 4:00 pm Discussion and closing remarks Content Introduction Beth McClenaghan & Vesa Peuraniemi Overview of processing methods for recovery of indicator minerals from sediment and bedrock samples M. Beth McClenaghan 1 Indicator minerals in diamond exploration: A case study from eastern Finnmark, Arkhangelsk and the Devonian Belt (Estonia, Lithuania, Novgorod and Pskov) Pavel Kepezhinskas 7 Exploring for RE and REE mineralization using indicator minerals Marja Lehtonen, Jukka Laukkanen & Pertti Sarala 13 Placer gold microchemistry in conjunction with mineralogy and mineral chemistry of heavy mineral concentrates to characterize bedrock sources Norman Moles & Rob Chapman 19 Applicability of sulphide and sulphate minerals in heavy mineral studies Vesa Peuraniemi & Tiina Eskola 27 Application of iron-oxide discriminant diagrams in mineral exploration Georges Beaudoin, Céline Dupuis, Beth McClenaghan, Jennifer Blain & Isabelle McMartin 35 Exploration case study using indicator minerals in till at the giant Pebble porphyry Cu-Au-Mo deposit, southwest Alaska, USA Robert G. Eppinger, Karen D. Kelley, David L. Fey, Stuart A. Giles & Steven M. Smith 41 Heavy mineral assemblages in Devonian sandstones and Quaternary sediments in Latvia Vija Hodireva & Denis Korpechkov 49 Kimberlite indicator mineral-based diamond exploration program in Karelia, northwest Russia Vladimir Ushkov 57 Indicator mineral signatures of magmatic Ni-Cu deposits, Thompson Nickel Belt, central Canada M.B. McClenaghan, S.A. Averill, I.M. Kjarsgaard, D. Layton-Matthews & G. Matile 67 Indicator Mineral Methods in Mineral Exploration, Workshop 3, 1-6. 25th International Applied Geochemistry Symposium The concentration of heavy minerals and recovery of indica- tor minerals from surficial sediment is one of the oldest explo- ration methods, being first applied to stream sediments in Roman times. The application of indicator mineral methods to mineral exploration has expanded and developed significantly over the past two decades. They are now used around the world to explore for a broad spectrum of deposit types includ- ing kimberlites (diamonds), lode gold, magmatic Ni-Cu-PGE, metamorphosed volcanogenic massive sulphides (VMS), por- phyry Cu, uranium, tin, tungsten, and rare metals (e.g. Averill 2001). Indicator minerals, including ore, accessory and alter- ation minerals, are usually sparsely distributed in their host rocks. Indicator minerals may be sparser in derived sediments, thus sediment samples must be concentrated in order to recover and examine them. Most indicator minerals have a moderate to high specific gravity, thus most processing tech- niques concentrate indicator minerals using some method of density separation, often in combination with sizing and/or magnetic separations. The presence of specific indicator min- erals in unconsolidated sediments provides evidence of a bedrock source in the provenance region and in some cases, the chemical composition of the minerals is associated with the ore grade of the bedrock source. As few as one sand-sized grain of a particular indicator mineral in a 10 kg sample may be significant. To recover such potentially small quantities (equiv- alent to ppb) of indicator minerals, samples are processed to reduce the volumeof material that must be examined. In reducing the volume of material, processing techniques must be able to retain the indicator mineral(s) and do so without contaminating the sample, without losing indicator minerals, and at a reasonable cost. Indicator minerals can be recovered from a variety of sam- ple media, including stream, alluvial, glacial, beach or eolian sediments and residual soils. They are also recovered from weathered and fresh bedrock as well as mineralized float. The combinations of processing techniques used by exploration companies or government agencies for recovering indicator minerals are quite variable (e.g. Gregory & White 1989; Peuraniemi 1990; Davison 1993; Towie & Seet 1995; Chernet et al. 1999; McClenaghan et al. 1999). These workshop notes are a summary of a more detailed paper describing common pro- cessing methods used to reduce sample weight, concentrate heavy minerals, and recover indicator minerals (Fig. 1) (McClenaghan in press). The methods used will depend on the commodities being sought as well as cost per sample. Most oxide and silicate indicator minerals are medium to coarse sand sized (0.25 to 2.0 mm). Thus, concentration techniques that recover the sand-sized heavy minerals can be used. In contrast, approximately 90% of gold grains, platinum group minerals (PGM) and sulphide minerals are silt sized (<0.063 mm), thus concentration of these indicators requires a preconcentration technique that includes recovery of the silt- as well as the sand- sized fractions. SAMPLE WEIGHT The weights of material collected for indicator mineral stud- ies will depend on the type of surficial sediment collected, the grain-size characteristics of the sample material, the commod- ity being sought and shipping costs (Table 1). For example, in glaciated terrain clay-rich till samples may be as much as 20 to 30 kg (or more) in order to recover a sufficient weight of sand- sized heavy minerals (Table 2 - #5) (e.g. Spirito et al. 2011). Coarse-grained silty sand till, typical of shield terrain, requires smaller (10 to 15 kg) samples because it contains more sand- sized material in the matrix (Table 2- # 1 to 4) (Spirito et al. 2011). Alluvial sand and gravel samples collected for recovery of porphyry Cu indicator minerals (PCIM) need only be ~0.5 kg because porphyry Cu alteration systems are large and rich in indicator minerals (Averill 2007). Bedrock and float samples usually vary from 1 to 10 kg. Overview of processing methods for recovery of indicator minerals from sediment and bedrock samples M. Beth McClenaghan Geological Survey of Canada, 601 Booth Street, Ottawa, Ontario, Canada K1A 0E8 (email: bmcclena@nrcan.gc.ca) Final concentration Lithology examination >2 mm or >1 mm Indicator Mineral Identification: Bulk sediment sample: 10 to 40 kg Heavy Fraction: Ferromagnetic Separation Nonferromagnetic fraction: Dry sieve to specific size fractions Sieve <2 mm or <1mm Preconcentration jig, spiral, shaking table, Knelson Concentrator, DMS, or pan 3 kg split for geochemical analysis & archive heavy liquids, and/or magstream Magnetic fraction: Examine or store 2. Chemical analysis: electron microprobe, LA-ICP-MS, Ion microprobe Indicator mineral selection Store under-/over- sized fractions 1. Examine & photograph < 2mm Fig. 1. Generalized flow sheet showing the steps in sample process- ing that are used to reduce sample weight, concentrate heavy miner- als, and recover indicator minerals. 2 M.B. McClenaghan BEDROCK PREPARATION Bedrock or float (mineralized boulders) samples often need to be disaggregated or crushed prior to processing to reduce rock fragment/mineral grain size to <2 mm. Electric pulse disag- gregation (EPD) using an electric current from a high-voltage power source in a water bath is an efficient means of liberating mineral grains from rock (Cabri et al. 2008). The major advan- tage of this method is that individual mineral grains can be recovered in their original shape and form regardless of grain size. Conventional rock crushers may also be used, however, they are more difficult to clean between samples and thus pose a higher risk of cross contamination, often break rock frag- ments across grain boundaries, and mark/damage grains as they are liberated. Barren quartz should be disaggregated or crushed as a blank between routine rock samples to reduce and monitor contamination. PRECONCENTRATION If sample shipping costs are an issue, samples may be partly processed in the field to reduce the weight of material shipped to the processing laboratory. Samples may be sieved to remove the coarse (>1 or >2 mm) fraction, which may reduce weights by a few % to 30% (e.g. Table 2-columns B-C). Preconcentrating, using a pan, jig, sluice box or Knelson con- centrator, also may be carried out in the field to further reduce the weight of material to be shipped. Preconcentrates may be examined in the field, significantly reducing the time to obtain results for follow up. However, preconcentraing in the field can itself be expensive and time consuming and the available meth- ods may not provide optimal recovery of the indicator miner- als of interest. Field setup of concentrating equipment may be more rudimentary than at the processing laboratory, thus extra care is required to avoid cross contamination or material lost during the pre-concentration procedure completed in the field. Whether sieved off in the field or in the laboratory, the coarse >2 mm fraction may be examined to provide additional information about sample provenance and transport distance. The <2 (or <1 mm) fraction is preconcentrated most com- monly using sieving and/or density methods (e.g. jig, shaking table, spiral, dense media separator, pan, Knelson concentra- Target Typical Sample Weight (kg) Table Micropan Ferro- magnetic separation? Ferro- magnetic separation? A. Sediment Samples Gold 10 Single Yes 3.3 Yes Kimberlite 10-30 Double No 3.2 Yes Massive sulphides (Ni-Cu-PGE, BHT, VMS, IOCG, MVT, skarn) 10 Single Yes (PGM only) 3.2 Yes Porphyry Cu 0.5 No No 2.8, 3.2 Yes Uranium 10 Single Yes 3.3 Yes Heavy mineral sands (grade evaluation) 20 Triple No 3.3 Yes Tampering (investigation) Variable Optional Yes 3.3 Yes B. Rock Samples Gold, PGE, base metals 1 Optional Yes 3.3 Yes Kimberlite 1-10 Optional No 3.2 Yes Tampering (investigation) 1 No Yes 3.3 Yes Required Separations latot:AerutxeTnoitacoL elpmas thgiew )gk( :B thgiew mm2> stsalC )gk( thgiew:C tupelpmas ssorca gnikahs )gk(elbat thgiew:D elbatgnikahs etartnecnoc )g(decudorp thgiew:E yvaeH diuqiL thgiL )g(noitcarf thgiew:F citengam noitcarf )g( -nonthgiew:G yvaehgam larenim )g(etartnecnoc mm0.2-52.0 9.744.635.4019.51010.210.30.51llitdnasytlistleBiNnospmohT.1 9.810.316.2041.52114.96.50.51llitydnasyrubduS.2 1.822.58.9131.3535.93.28.11llitdnasytlispmacdloGsnimmiT.3 8.530.220.7737.8346.82.18.9llitdnasytlisetilrebmikBelpirT.4 5.116.52.532,10.703,10.564.24.76llityeyalcatreblAnrehtroN.5 Table 1. Examples of variation in sample weight and processing procedures with sample and target type at Overburden Drilling Management Ltd.’s heavy mineral processing laboratory (Averill & Huneault 2006). Table 2. Weight of each fraction generated by a combination of tabling and heavy liquid separation to reduce till sample weight, concentrate heavy minerals, and recover indicator minerals: A) initial sample weight; B) sieving off <2 mm; C) & D) tabling; E) heavy liquid separation; F) magnetic separation; G) final heavy mineral concentrate weight. Till samples are from 1) the South Pit of the Thompson Ni Mine, Thompson, Manitoba; 2) Broken Hammer Cu-PGE deposit, Sudbury, Ontario; 3) PamourMine, Timmins, Ontario; 4) Triple B kimberlite, Lake Timiskaming field, Ontario; and 5) Buffalo Head Hills, northern Alberta. 3Overview of processing methods for recovery of indicator minerals from sediment and bedrock samples tor) to reduce the weight of material to be examined without losing indicator minerals. Some of the more common precon- centration techniques are described below. Panning Panning is the oldest method used to recover indicator miner- als, primarily for gold and PGM. Sediment is placed in a pan and shaken sideways in circular motion while being held just under water; heavy minerals sink to the pan bottom and light minerals rise and spill out over the top (Silva 1986; English et al. 1987; Ballantyne & Harris 1997). Pans are of various shapes (flat bottomed or conical) and sizes, and can be made out of plastic, metal or wood. The advantages of this technique include that it can be a field or laboratory-based operation, is inexpensive in terms of equipment costs, and if used in the field it reduces sample shipping weight and thus cost. Panning is often used in combination with other preconcentration methods to recover silt-sized precious metal grains (e.g. Grant et al. 1991; Leake et al. 1991, 1998; Ballantyne & Harris 1997; Wierchowiec 2002). The disadvantages of this method are that it is slow, is highly dependent on the experience and skill of the operator and therefore requires consistent personnel to per- form the panning. It is considered to be a rough concentrating method when used in the field and is followed up with further laboratory-based concentration techniques (Stendal & Theobald 1994). Tabling Preconcentration using a shaking (Wilfley) table is one of the oldest methods for concentrating and separating heavy miner- als on the basis of density. It recovers silt- to coarse sand-sized heavy minerals for a broad spectrum of commodities includ- ing diamonds, precious and base metals, and uranium (Averill & Huneault 2006). A brief description of the method is sum- marized below from Sivamohan & Forssberg (1985), Stewart (1986), and Silva (1986). The table consists of a deck covered with up to 1 cm high riffles covering over half the surface. A motor mounted on one end drives a small arm that shakes the table along its length. A slurry of <2.0 mm sample material is put across a shaking table to prepare a preconcentrate. If kimberlite indicators are tar- geted, the sample is tabled twice to ensure higher recovery of the key lower density minerals (Cr-diopside and forsteritic olivine) and the coarsest grains. The advantages of this method are its moderate cost, ability to recover indicator minerals for a broad spectrum of commodities, and ability to recover silt- as well as sand-sized indicators. It is a well established method for the recovery of precious metal mineral grains as well as kim- berlite indicator minerals (e.g. English et al. 1987; McClenaghan et al. 1998; 2004). The disadvantages of this method include the loss of some coarse heavy minerals during tabling, the longer time required to process each sample, and that the tabling procedure is dependent on the skill of the operator. Dense Media Separator A gravity method used to preconcentrate kimberlite indicator minerals is the micro-scale dense media separator (DMS). An overview of this method is summarized below from Baumgartner (2006). Heavy mineral concentration is carried out using a gravity- fed high-pressure cyclone. The <1 mm fraction of a sample is mixed with fine-grained ferrosilicon (FeSi) to produce a slurry that has a controlled density. The slurry is fed into a cyclone where the grains travel radially and helically, forcing the heav- ier particles toward the wall of the cyclone and the lighter par- ticles toward the centre. The lighter and heavier particles exit the cyclone through different holes, with the light fraction dis- carded and the heavy fraction collected on a 0.25 or 0.3 mm screen. The heavy mineral concentrate is collected on a 0.25 mm screen and is then dried and screened to remove residual FeSi. A Tromp curve is used to define the efficiency and preci- sion of the DMS separation. The DMS is calibrated to recover the common kimberlite indicator minerals that have a specific gravity (SG) >3.1 : pyrope garnet, chrome-spinel, Mg-ilmenite, Cr-diopside, forsteritic olivine and diamond. It is tested using synthetic density tracers before processing samples. The den- sity settings and cut points are checked once per day. The advantages of the micro DMS system are that it is fast, less sus- ceptible to sample contamination than other heavy mineral concentrating techniques and not operator dependent. The method, however, is more expensive than other methods described here and it does not allow for the recovery of silt- sized precious and base metal indicator minerals. Knelson concentrator The Knelson concentrator is a fluidized centrifugal separator that was originally designed for concentrating gold and plat- inum from placer and bedrock samples. However, in recent years it has also been used to recover kimberlite indicator min- erals from sediment samples (e.g. Chernet et al. 1999; Lehtonen et al. 2005). The concentrator can handle particle sizes from >10 microns up to a maximum of 6 mm. The general pro- cessing procedure is summarized below from the Knelson con- centrator website (http://www.knelsongravitysolutions.com). Briefly, water is introduced into a concentrate cone through a series of holes in rings on the side of the cone. The sample slurry is then introduced into the concentrate cone from a tube at the top. When the slurry reaches the bottom of the cone, it is forced outward and up the cone wall by centrifugal force from the spinning cone. The slurry fills each ring on the inside of the cone wall to capacity to create a concentrating bed. High specific gravity particles are captured in the rings and retained in the concentrating cone. At the end of the concentrate cycle, concentrates are flushed from the cone into the sample collec- tor. The advantages of the Knelson concentrator are that it is fast, inexpensive, and can be mobilized to the field to reduce the weight of material to be shipped to the laboratory. However, recovery of kimberlite indicator minerals from silt- poor material, such as esker sand or stream sediments, is diffi- cult due to the absence of fine-grained material to keep the slurry in suspension (Chernet et al. 1999). Knelson concentra- tors are optimal for recovery of gold and PGM. Spiral concentrator Heavy minerals can be recovered using a rotary spiral concen- trator that consists of a flat circular stainless steel bowl with rubber ribs that spiral inward, a detailed description of which is reported by Silva (1986). A spiral concentrator is mounted on a frame so it can be tilted and has a water wash bar extend- 4 M.B. McClenaghan ing laterally from one side of the bowl to the centre. As the bowl spins, water is sprayed from the bar and heavy mineral grains move up and inward along the spirals to the central opening where they are collected in a container behind bowl. Water washes light minerals down to the bottom bowl. The heaviest minerals are recovered first. The advantages of the spiral concentrator are that it can be field based and thus reduce sample weight to be shipped, it is inexpensive to acquire and operate, it is fast if the material is sandy, and it recovers indicator minerals across a broad size range from silt- to sand- size grains. The method, however, is dependent on experience and skill of the operator, the lower density threshold is vari- able, there is some loss of heavy minerals and the method is slow if the sample is clay-rich. It is used mainly for gold recov- ery (e.g. Maurice & Mercier 1986; Silva 1986; Sarala etal. 2009) but in the past 10 years it also has been used for the recovery of kimberlite indicator minerals (e.g. Sarala & Peuraniemi 2007). Jigs Jigging is one of the oldest gravity concentration methods and separates heavy minerals based on differential settling veloci- ties of mineral grains in water (Stendal & Theobald 1994). Jigging is performed by hand or by mechanically jerking a par- tially filled screen of material up and down underwater for sev- eral minutes. While submersed in water, mineral grains separate through suspension and gravity effects into layers of varying specific gravity. Heavier grains concentrate on the surface of the screen, with the heaviest generally concentrated towards the centre of the screen forming an ‘eye’. Very heavy minerals, such as ilmenite and magnetite, will be found at the very cen- tre of the screen and lighter heavy minerals, such as garnet and pyroxene, will concentrate at the periphery of the eye. Diamonds tend to concentrate towards the centre despite their moderate specific gravity (SG 3.51). A spoon is used to remove the heavy minerals in the eye for more detailed examination. For optimal recovery, the jig tailings should be re-jigged 2 to 3 times until no eye exists. The method is typically used for recovery of gold (e.g. Silva 1986) and kimberlite indicator min- erals (Muggeridge 1995). The advantages of using a jig are that it can be field based and thus reduce sample weight to be shipped, is inexpensive to operate, is relatively fast and works best for fine to coarse sand-sized grains. It is best used in a fixed, laboratory-based setting with an experienced operator. FINAL CONCENTRATION Heavy liquid separation A preconcentrate is usually further refined using heavy liquids of a precise density to further reduce the size of the concen- trate prior to heavy mineral selection (Table 2-column E). Heavy liquid separation provides a sharp separation between heavy (sink) and light minerals (float) at an exact known den- sity. It is slow and expensive and therefore not economical for large volumes of sample material, hence the preconcentration procedures described above that are used to prepare a precon- centrate before this step (Stendal & Theobald 1994). The most common heavy liquids used include methylene iodide (MI) with a SG of 3.3 and tetrabromoethane (TBE) or the low-tox- icity heavy liquid lithium heteropolytungstates (LST) both with SG of 2.9. The density required of the heavy liquid will depend on the indicator minerals being sought. Some laboratories use a combination of both heavy liquids, separating first using the lower density heavy liquid at about SG 2.9 to reduce the vol- ume of material to be further separated at SG 3.2 or 3.3. (e.g. de Souza 2006; Le Couteur & McLeod 2006; Mircea 2006). The recovery of kimberlite and magmatic Ni-Cu-PGE indica- tor minerals requires heavy liquid separation at SG 3.2 using dilute methylene iodide to include the lowest density indicators Cr-diopside and forsteritic olivine. Recovery of porphyry Cu indicator minerals requires separation at SG 2.8 to 3.2 to recover the mid-density indicators tourmaline (dravite), alunite, jarosite, and turquoise (Averill 2007). Some indicator minerals, such as apatite and fluorite, are of intermediate density but are recovered mainly from the mid-density rather than the heavy fraction. Magnetic separation Magnetic separation may be used to further refine heavy min- eral concentrates and reduce concentrate volume for picking of mineral species with specific magnetic susceptibilities (Towie & Seet 1995). The most common magnetic separation is splitting the ferromagnetic from the nonferromagnetic fraction because the ferromagnetic minerals can comprise a considerable por- tion of the concentrate (e.g. Table 2-column F). Removing the ferromagnetic minerals decreases concentrate size prior to indicator mineral selection and removes any steel contaminants derived, in most instances, from sampling tools. The ferro- magnetic fraction may then be (1) set aside, (2) examined to determine the abundance and mineral chemistry of magnetite (e.g. Beaudoin et al. 2011), pyrrhotite or magnetic Mg-ilmenite, as is the case for some kimberlites (e.g. McClenaghan et al. 1998), or (3) analyzed geochemically (e.g. Theobald et al. 1967). A hand magnet or plunger magnet is most commonly used to carry out this separation. A specific size fraction of the non-ferromagnetic heavy mineral fraction may be further separated electromagnetically into fractions with different paramagnetic characteristics to help reduce the volume of material to be examined for indica- tor minerals (Averill & Huneault 2006). Minerals such as dia- mond are nonparamagnetic, pyrope garnet, eclogitic garnet, Cr-diopside and forsteritic olivine are nonparamagnetic to weakly paramagnetic, and Cr-spinel and Mg-ilmenite are mod- erately to strongly paramagnetic (see Table 1 in McClenaghan & Kjarsgaard 2007). If the non- or paramagnetic portion of the concentrate contains a significant amount of almandine garnet it may be processed through a magstream separator to separate the orange almandine from similar looking eclogitic or pyrope garnets. Magstream separation divides the concentrate into (1) a fraction containing most of the silicates (e.g. pyrope and eclogitic garnet) and no almandine, and (2) a fraction con- taining ilmenite, chromite and other moderately magnetic min- erals such as almandine (Baumgartner 2006). INDICATOR MINERAL SELECTION AND EXAMINATION The non-ferromagnetic fraction is commonly sieved into two or three (e.g. 0.25-0.5 mm, 0.5-1.0 mm and 1.0-2.0 mm) size fractions for picking of indicator minerals, however the final size range will depend on the commodity sought. For example, kimberlite indicator minerals are most abundant in the 0.25-0.5 5Overview of processing methods for recovery of indicator minerals from sediment and bedrock samples mm fraction (McClenaghan & Kjarsgaard 2007) and thus to maximize recovery and minimize counting time and cost, this finest size fraction is most commonly picked. Indicator minerals are selected from non-ferromagnetic heavy mineral concentrates during a visual scan, in most cases, of the finer size (e.g. 0.25-0.5 mm, 0.3-0.5 mm or 0.25-0.86 mm) fractions using a binocular microscope. The grains are counted and a selection of grains are removed from the sam- ple for analysis using an electron microprobe (EMP) to con- firm their identification. Methods for examining a sample for counting/picking vary from rolling conveyor belts to dishes/paper marked with lines or grids. If a concentrate is unusually large, then a split is examined and the indicator min- eral counts are normalized to the total weight of the concen- trate. If a split is picked, the weight of the split and the total weight should both be recorded. Not all grains counted in a sample will be removed for EMP analyses. If this is the case, the total number of grains counted and the number of grains removed should both be recorded. Indicator minerals are visually identified in concentrates on the basis of colour, crystal habit and surface textures, which may include features such as kelyphite rims and orange peel textures on kimberlitic garnets (Garvie 2003; McClenaghan & Kjarsgaard 2007). Scheelite and zircon in a concentrate may be counted under short-wave ultraviolet light. Gold and PGM grains may be panned from concentrates that were prepared in such a way that the silt-sized fraction has been retained (e.g. tabling). The grains may be counted and classified with the aid of optical or scanning electron microscopy. Commonly, gold grains are classified according to their shape/degree of wear (e.g. DiLabio 1990, Averill 2001), which can provide informa- tion about relative transport distances (McClenaghan & Cabriin press). INDICATOR MINERAL CHEMISTRY Mineral chemical analysis by EMP, scanning electron micro- probe (SEM), laser ablation-ICP-MS, or secondary ion mass spectrometry (SIMS) may be carried out to determine major, minor and trace element contents of specific indicator miner- als because mineral chemistry is used to confirm identity, establish mineral paragenesis, and in some cases deposit grade (e.g., Ramsden et al. 1999; Belousova et al. 2002; Scott 2003; Heimann et al. 2005). For example, kimberlite indicator miner- als are characterized by a specific range of compositions that reflect their mantle source and diamond grade (e.g. Fipke et al. 1995; Schulze 1997; Grütter et al. 2004; Wyatt et al. 2004). Gold, PGM and sulphide grains may be analyzed to determine their trace element chemistry or isotopic compositions (e.g. Grant et al. 1991; Leake et al. 1998; Chapman et al. 2009). Prior to indi- cator mineral grains being selected from a heavy mineral con- centrate, newer techniques such as mineral liberation analysis (MLA), computer-controlled scanning electron microscopy (CCSEM), or quantitative evaluation of materials by scanning electron microscopy (QEMSCAN) may provide quantitative mineralogical analysis and identification of indicator minerals in a portion of the heavy mineral concentrate that has been prepared as a polished epoxy grain mount, in the 0.25 to 2.0 mm fraction of the rarely examined <0.25 mm fraction. These methods can be used to identify indicator minerals of interest and prioritize grains for further detailed and more costly EMP analysis, thus reducing EMP analytical costs. The cost per sam- ple for these new techniques is, in general, more expensive than conventional methods. QUALITY CONTROL Project geologists may use a combination of blank samples (no indicator minerals), spiked samples (known quantity of specific indicator mineral species), and field duplicates, as well as repicking of 10% of the heavy mineral concentrates to moni- tor a laboratory’s potential for sample contamination and qual- ity of mineral grain selection. In addition, heavy mineral pro- cessing and identification laboratories can be asked to report their own quality control monitoring procedures and test results. Quality assurance and control measures are being implemented at the Geological Survey of Canada for projects using indicator minerals (Spirito et al. 2011). SUMMARY These workshop notes describe some of the procedures avail- able for processing surficial media and rocks to recover indica- tor minerals for mineral exploration. The processing method used will depend on sample media, commodities being sought, budget, bedrock and surficial geology of the survey area, and processing methods used for previous batches. When report- ing indicator mineral results in company assessment files, gov- ernment reports, or scientific papers, it is helpful to report the laboratory name, processing methods used, and sample weights. Monitoring of quality control is essential at each stage in the processing, picking, and analytical procedures described here and should be monitored both by the processing labora- tories and clients. Geologists are encouraged to visit process- ing and picking laboratories so that they have a clear under- standing of the procedures being used and can discuss cus- tomizations needed for specific sample batches. ACLMPW;EDGEMENTS S. A. Averill of Overburden Drilling Management Ltd., T. Nowicki and M. Baumgartner of Mineral Services Canada, and L. 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Morphology and chemistry of placer gold grains – indicators of the origin of the placers: an example from the East Sudetic Foreland, Poland. Acta Geologica Polonica, 52, 563-576. WYATT, B.A., BAUMGARTNER, M., ANCKAR, E. & GRÜTTER, H. 2004. Compositional classification of kimberlitic and non-kimberlitic ilmenite. Lithos, 77, 819-840. Indicator Mineral Methods in Mineral Exploration, Workshop 3, 7-11. 25th International Applied Geochemistry Symposium Indicator minerals have been successfully used in diamond exploration for more than 50 years worldwide. Kimberlites contain a rich mineral inventory that includes olivine, peri- dotitic and eclogitic garnets, chrome spinel, chrome diopside, Mg-ilmenite, enstatite, phlogopite, and periclase among others. Kimberlite indicator minerals (KIMs) for the purposes of this presentation can be subdivided into two groups: 1) typical or common and 2) exotic. Common kimberlite indicator minerals belong to two mantle assemblages – peridotitic and eclogitic (Stachel & Harris 2008; Gurney et al. 2010). Peridotitic KIMs include pyrope garnet (of lherzolitic or G9 and harzburigitic- dunitic or G10 chemical affinity), Mg-rich ilmenite, Cr-rich spinel, Cr-rich diopside, enstatite, and forsteritic olivine. Eclogitic indicator minerals primarily consist of eclogitic (Na- rich) garnet and Na-rich omphacitic clinopyroxene (commonly with elevated K contents reflecting the high pressures involved in their formation). Exotic kimberlite minerals include such phases as corundum and uvarovite (Ca-Cr-rich garnet). Corundum is present in kimberlites and as inclusions in dia- monds but also occurs in peraluminous metamorphic rocks and peralkaline syenites and pegmatites.Corundum – espe- cially with elevated Mg, Cr, Ni, Ti, and Fe concentrations – is an important indicator mineral in kimberlite exploration because it is most probably derived from eclogite xenoliths fre- quently carried by kimberlite melts (Hutchinson et al. 2004). Kimberlite-borne eclogitic xenoliths are commonly associated with impressive diamond grades - they average 14,000 cpt, fre- quently up to 90,000 cpt (Spetsius 2004). One eclogitic xeno- lith (66 grams) from Udahcnaya Pipe in Siberia contains 74 microdiamonds implying grade of 144,000 cpt. Uvarovite essentially is a crustal mineral, but when found in kimberlites is positively correlated with diamond grade of indi- vidual pipes (as exemplified by several pipes in Siberia and Canada). Uvarovite is typically associated with chromites and Cr-rich ore formations including certain skarns, but in the absence of such rock formations within certain exploration territory, it can be successfully used – together with other KIMs – to locate primary diamond sources. Another potential “exotic” indicator mineral of kimberlitic assemblage is moissanite (SiC), which has been documented in kimberlites and glacial and alluvial sediments from Siberia, Canada, China, Western Australia, Tersky Bereg of Kola Peninsula, and Latvia (Hodireva et al. 2003; Shiryaev et al. 2011). Moissanite has also been reported as inclusions in dia- monds from Fuxian kimberlite in China (Leung 1990). Besides chemical and optical identification of kimberlite indicator minerals, detailed studies of their crystal shape and other surficial features (such as cleavage, surface sculptures, formation of secondary alteration production such as kelyphitic rims on garnets) are of great importance in diamond exploration, specifically for estimating the mode and distances of transport of these indicator minerals. The purpose of this mineralogical exercise ultimately is determination of proximity of primary magmatic sources of kimberlitic indicator minerals, which means the ground locations of kimberlitic pipes. Presence of KIMs with so-called “diamond chemistry” (e.g. minerals formed under P-T-Of conditions compatible with dia- mond formation and stabilization in cratonic lithosphere) is crucial for location of diamond-bearing kimberlite pipes as opposed to barren diatremes. Kimberlitt AS’s exploration in eastern Finnmark established the presence of olivines and chrome diopsides with diamond window chemistry as well as corundum, uvarovite, and Mg- spinel in till, lake, and river sediments. Some diamond window KIMs in eastern Finnmark show complete preservation of such crystal features as cleavage, which suggests derivation from local kimberlite sources (within <1 km). These data are compared with exploration results from the Arkhangelsk diamond province and the Devonian Belt of the Eastern European Craton (Lithuania, Estonia, Novgorod, and Pskov) and possible implications for location of diamondiferous kim- berlitic pipes through regional exploration are discussed. EASTERN FINNMARK (NORWAY) Eastern Finnmark is underlain by thick Precambrian continen- tal crust which, on the basis of our recent geochronological studies, reveals complex crustal evolution history. Oldest inher- ited zircon grains from basement grey gneisses yield Early Archean ages of 3.69 and 3.2 Ga, suggesting the presence of a very old crustal component under this part of the East European craton. The peak of crustal production in Eastern Finnmark happened around 2.8-2.9 Ga, which was followed by another episode of thermal re-activation, high-grade metamor- phism, and granitic magmatism at 2.5 Ga. This crustal chronol- ogy suggests that Eastern Finnmark retains a protracted his- tory of evolution of mature continental crust that is broadly similar to terrains in other Northern Atlantic cratons, such as Finland, Greenland, and Canada. Kimberlitt AS carried a reconnaissance sediment sampling survey within a part of Eastern Finnmark covering an area over 3,000 km2. Several populations of indicator minerals have been subsequently recovered including olivines, chrome diop- sides, Mg-spinel, corundum, and uvarovite. Olivines have Fo contents of 86 to 92 and elevated Ni contents of up to 0.6 wt.%, comparable with those typical of kimberlitic olivines (Kamenetsky et al. 2008). Chrome diopsides display low-Al (under 1 wt.% of Al2O3) and Cr contents of 1.5 wt.%. Some clinopyroxenes also have elevated Na concentrations coupled with high Cr contents, which is typical of mantle-derived diop- sides. These chrome diopsides from Eastern Finnmark plot into a field of diamond inclusion clinopyroxenes on a Cr2O3- Indicator minerals in diamond exploration: A case study from eastern Finnmark, Arkhangelsk and the Devonian Belt (Estonia, Lithuania, Novgorod, and Pskov) Pavel Kepezhinskas Kimberlitt AS, Tolbugatta 24, Oslo, Norway (e-mail: pavel_k7@yahoo.com) Al2O3 discrimination diagram. Corundum exhibits high Cr, Fe, Mg, and Ni contents, consistent with their kimberlitic provenance (Hutchison et al. 2004). So far the regional miner- alogical signature in Eastern Finnmark is chrome diopside>olivine>>corundum>Mg-spinel>uvarovite. However, it is the appearance of the KIM grains that might be helpful in unlocking the diamond potential of Eastern Finnmark. Fairly significant populations (locally up to 20-30 percent of the total number of heavy minerals recovered from till or river sediment) of indicator mineral grains from Eastern Finnmark retain primary magmatic crystal habits and are characterized by a minimal degree of chemical abrasion and physical wear. Some chrome diopsides show features such as mineral cleavage and some forms or sculptures, which are indicative of growth in igneous melts (Fig. 1), suggest of very limited transport in fluvio-glacial systems, and possible origin from local kimberlite sources. Cleavage is a particularly important diagnostic feature in relation to localization of primary magmatic sources of these clinopyroxene grains since it can not be preserved in diopside grains during transport by water or ice over distances of more than several hundreds of metres. Other chrome diop- sides exhibit various degrees of chemical abrasion (Fig. 2) that are indicative of more complicated transport histories and advanced travel distances. Magnesian spinel shown in Figure 3 has retained its original octahedral crystal shape and magmatic crystal growth features, which – as in the case of the chrome diopside grain shown in Figure 1 – is also an indication of its derivation from local magmatic sources. ARKHANGELSK The Arkhangelsk region of northwest Russia is underlain by Precambrian continental crust composed of Late Archean to Proterozoic granulites, gneisses, granites, and greenstone belts (terrains). Mantle conditions beneath the Arkhangelsk region are comparable to classic diamondiferous cratons worldwide, such as the Kaapvaal craton in South Africa and the Slave cra- ton in Canada. Single clinopyroxene thermobarometry defines a cool continental geotherm similar to the 36 mW/m2 geot- herm calculated by Kukkonen et al. (2003) for the 600 million year old Karelian craton. These mantle conditions are favourable for diamond formation within the Arkhangelsk mantle at depths of 110 to 224 kilometres (corresponding to the diamond stability field) and are further confirmed by geo- chemical signatures of pyropes and chromites from a high- grade Arkhangelskaya pipe in the Lomonosov diamond deposit (Lehtonen et al. 2009). Kostrovitsky et al. (2004) report pressures of 28 to 68 kbars derived from a megacryst suite (garnet, clinopyroxene, Mg-ilmenite, phlogopite, and garnet- pyroxene intergrowths) in the diamondiferous Grib pipe, which again is supportive of kimberlites sampling diamond- rich mantle withina cool cratonic keel beneath the Arkhangelsk region. Low-hematite content of ilmenite megacrysts suggest low oxygen fugacity and overall reducing conditions in the mantle during its formation, which indicates an environment favourable for diamond preservation (Kostrovitsky et al. 2004). Indicator mineral studies in the northern part of the Arkhangelsk region are abundant and have led in the past to successful discoveries of more than 30 kimberlite pipes, seven of which – 6 pipes of Lomonosov kimberlite cluster and the 8 P. Kepezhinskas Fig. 1. Chrome diopside from Eastern Finnmark with primary mag- matic features (such as cleavage) indicative of short transport distances (Jakobselv Target Area, sample 1083). Fig. 2. Partially resorbed and chemically altered chrome diopside sug- gesting a more complex transport history. Fig. 3. Unabraded Mg-spinel grain retaining primary magmatic features. 9 Grib pipe in the Verkhotina kimberlite field – carry economic diamond mineralization. These pipes include the spectacular Grib pipe with a net present value of 9.3 billion US dollars in the ground and a high-grade (0.85 to 1 cpt) Arkhangelskaya pipe within the Lomonosov kimberlite cluster that is currently being mined by the Russian diamond producer ALROSA. The regional study discussed in this presentation is focused on the central and southern Arkhangelsk region and was car- ried out in 2006 to 2008 by a now defunct private diamond explorer, Russian Diamonds plc. Abundant indicator minerals were collected within the Tokshenga property in the central Arkhangelsk region (Fig. 4). Indicator minerals are dominated by pyrope garnets (both G9 and G10 types), olivine (Fo content of 87 to 95, Ni content up to 0.4 wt.%), chromite, and low-Al, high-Cr clinopyroxene. Spatial distribution patterns, morphology of individual KIM grains combined with local ice-flow directions suggest the presence of kimberlitic sources within the western portion of this area (Fig. 4). Indicator minerals within the southern part of the Arkhangelsk region (Lachsky property) are dominated by pyrope garnets. Based on microprobe analyses of more than 70 grains collected from Quaternary river sediments, it appears that a vast majority of diamond grains have originated within the diamond stability field (Fig. 5). Co-variation of Cr2O3 and CaO in these garnets indicates that most of the grains are lher- zolitic G9 garnets with harzburgitic G10 garnets forming a subordinate but prominent population (Fig. 5), suggesting that kimberlite source rocks of these pyropes might be associated with diamond mineralization. Although some garnet grains Indicator minerals in diamond exploration: A case study from eastern Finnmark, Arkhangelsk and the Devonian Belt 110 Depth (m) to Target Pyrope (1-8 grains) Chromite (1-2 grains) CPX (1-50 grains) National Park Carboniferous Vendian N Ultramafics & Greenstone Belts Devonian KIM Distrubution Archean 0 30km Tokshenga License Quaternary Ice Direction Olivine (1-3 grains) Fig. 4. Distribution of indicator minerals in central part of the Arkhangelsk region (Russian Federation). Fig. 5. Chemical composition and crystal morphology of indicator minerals in southern part of the Arkhangelsk region (Russian Federation). show clear signs of chemical abrasion (pitting) and physical wear (extensive rounding) indicative of large transport dis- tances, a number of low-Ca pyropes exhibit angular forms with well preserved elements of original chemical textures, suggesting that they were derived from local kimberlite sources. THE DEVONIAN BELT – BALTIC STATES The Baltic States are located within a geological feature known as the Devonian Belt, which is essentially a significant area within the western portion of East European Craton domi- nated by Devonian sedimentary cover. Kimberlite indicator minerals were reported earlier from Latvia (Hodireva et al. 2003) and were later discovered by us in Lithuania and Estonia under the auspices of a regional reconnaissance study funded by De Beers in the early 1990s. Indicator minerals were recovered from both Devonian and Quaternary sediments in Lithuania. KIM populations are clearly dominated by chrome spinels with subordinate garnets and minor picroilmenite (chrome spinel>>garnet>Mg- ilmenite). Chrome spinels form a typical “regional array” on the Cr2O3-MgO discrimination plot with approximately 10 percent of all chemical analyses (185 analyses) plotting within or near the diamond inclusion field (Table 1). Garnets are dominated by lherzolitic compositions; however some border- line G10 chemistries have been also detected (Table 1). Magnesian ilmenites are characterized by fairly high MgO con- tents and are consistent with the overall derivation of Lithuanian indicator mineral suites from kimberlitic sources. Indicator minerals from Devonian sedimentary rocks (Skervele suite) are mostly heavily abraded, suggesting their processing through one or more secondary sedimentary collectors, while indicator grains from modern river sediments contain a healthy population (about 30 percent) of grains showing only minor chemical alteration or no signs of any significant transport at all. Indicator minerals in Estonia are less abundant compared to Lithuania, but it also might reflect some sampling bias (less samples collected in Estonia due to certain time limitations). Indicator mineral populations in modern river sediments are dominated by garnets with subordinate spinels. Several grains of corundum with elevated Ni contents (45-65 ppm) were also recovered. Garnets are mostly lherzolitic G9 and borderline G9/G10 varieties. Spinels have moderate to high chrome chemical compositions with elevated FeO contents and Fe/Mg ratios. Overall recovered indicator minerals in Estonia were interpreted as broadly kimberlitic in origin. However, most of the grains show extensive degrees of chemical abrasion and nearly total absence of primary magmatic features, which sug- gests to us that these indicator minerals were probably deliv- ered into modern river drainage from secondary sedimentary collectors of Devonian/Carboniferous/Permian and even possibly Paleogene/Neogene age and reconstruction of their transport distances and, hence, localization of primary kim- 10 P. Kepezhinskas garnet garnet garnet ilmenite spinel spinel spinel spinel garnet garnet spinel SiO2 40.94 40.11 41.2 n.d. n.d. n.d. n.d. n.d. 40.21 41.19 n.d. TiO2 0.63 0.52 0.26 47.05 0.09 0.0 0.03 0.0 0.3 0.26 0.18 Al2O3 20.55 20.11 20.55 0.22 4.63 7.09 8.43 4.55 19.21 19.22 6.57 C O 4 59 5 16 5 18 1 23 64 98 63 22 61 07 65 17 5 59 4 69 60 9 Oxide Lithuania Estonia Cr2O3 4.59 5.16 5.18 1.23 64.98 63.22 61.07 65.17 5.59 4.69 60.9 FeO 7.88 7.17 7.12 42.34 19.5 16.08 19.84 16.53 6.71 7.03 20.97 MnO 0.33 0.23 0.26 0.34 0.36 0.33 0.41 0.36 0.32 0.31 0.42 MgO 20.56 21.21 20.59 8.21 10.01 13.86 9.43 13.79 22.05 22.13 10.25 CaO 4.85 4.55 4.68 n.d. n.d. n.d. n.d. n.d. 4.78 4.46 n.d. Na2O 0.0 0.05 0.12 n.d. n.d. n.d. n.d. n.d. 0.21 0.12 n.d. Total 100.33 99.12 99.96 99.39 99.77 100.58 99.21 100.4 99.38 99.41 99.29 Note: n.d. - not determined Table 1 . Chemical composition of indicator minerals in modern sediments from Lithuania and Estonia. tenragtenragtenragenexoryponilcenexoryponilcetinemlietinemlietinemlitenragtenragtenrag OiS 2 .d.n.d.n.d.n71.1477.0436.04 93.55 92.0444.0410.2438.55 OiT 2 28.00.031.00.00.075.4470.4446.848.00.00.0 lA 2O3 35.6124.6121.7119.036.045.095.086.098.6128.6159.41 rC 2O3 10.961.0155.821.142.16.062.015.030.751.880.21 61.665.643.570.125.130.2495.6468.9317.740.761.7OeF 53.04.043.00.00.044.03.0064.084.03.0OnM 97.0282.0216.1294.6132.6196.777.884.887.9148.9110.91OgM 76.594.517.470.5253.52.d.n.d.n.d.n31.673.630.5OaC aN 2 .d.n.d.n.d.n86.094.0.d.n.d.n.d.n.d.n.d.n.d.nO26.9957.9918.9964.00163.00116.9985.00171.8949.9974.9961.99latoT denimretedton-.d.n:etoN edixO noigervoksPnoigerdorogvoN Table 2. Chemical composition of indicator minerals in modern sediments from Novgorod and Pskov regions of Russian Federation. 11 berlitic sources in reality represents an unrealistic, if not impossible, task. THE DEVONIAN BELT – NOVGOROD AND PSKOV REGIONS OF RUSSIAN FEDERATION Indicator minerals were reported in high concentrations (up to 300-500 grains per 20 litre sample) throughout the central European Russia (Novgorod, Pskov, and Tver regions). Diamonds – both unabraded cubic crystals and fragments – were also found in the Novgorod region in association with kimberlitic garnets and spinels (Table 2). Garnets are mostly chrome-rich pyropes, some with well developed kelyphitic rims, suggesting short transport distances and local kimberlitic sources. Other garnets show variable degrees of chemical abra- sion, suggesting complex transport history and possible resi- dence in one or more Paleozoic sedimentary collectors. Follow-up on several strong pyrope/chrome spinel indicator trains led to a discovery of a metakimberlite pipe in the central Novgorod region, however no information on its diamond content is available at this time. CONCLUSIONS The case studies presented above highlight the importance of regional and local surveys of indicator minerals in diamond exploration. Local geochemical signatures – predominance of certain minerals over other indicators – can be established through such surveys and can be used to characterize individ- ual kimberlite clusters or larger kimberlite provinces on a cra- ton scale. Not all traditional kimberlite indicator minerals – peridotitic and eclogitic garnets, chrome spinels, Mg-ilmenites, chrome diopsides, forsteritic olivines – should and can be pres- ent, but the presence of indicator minerals with diamond inclusion chemistry is essential for ultimate exploration suc- cess. Some kimberlite provinces, fields, and clusters are associ- ated with “exotic” indicator minerals, such as corundum (with elevated Cr, Ni, Fe, and Ti concentrations) and green Ca-Cr uvarovitic garnet, which can provide valuable information on the location of primary kimberlitic sources and even provide some possible insights into the potential diamond grade of these kimberlitic sources (e.g. uvarovite). Finally, crystallo- graphic appearance and degree of chemical alteration and physical wear (degree of rounding, preservation of primary crystallographic features, cleavage, original magmatic growth forms on crystal planes, kelyphitic rims on garnets, etc.) of kimberlite indicator minerals are important in deciphering of their transport histories, distances from primary sources, and potential residence in Phanerozoic secondary sedimentary col- lectors. All these factors are essential in ensuring that each and every diamond exploration effort leads to ultimate success, not ultimate failure. REFERENCES GURNEY, J.J., HELMSTAEDT, H.H., RICHARDSON, S.H. & SHIREY, S.B. 2010. Diamonds through time. Economic Geology, 105, 689-712. HODIREVA, V., KORPECHKOV, D., SAMBURG, N., & SAVVAITOV, A. 2003. Sources of kimberlitic minerals in clastic sediments of Latvia and some problems in the succession of formation of supposed kimberlites. Geologija, 42, 3-8. HOOD, C.T.S. & MCCANDLESS, T.E. 2004. Systematic variation in xenocryst mineral composition at the province scale, Buffalo Hills kimberlites, Alberta, Canada. Lithos, 77, 739-747. HUTCHINSON, M.T., NIXON, P.H. & HARLEY, S.L. 2004. Corundum inclusions in diamonds – discriminatory criteria and a corundum compositional dataset. Lithos, 77, 273-286. KAMENETSKY, V.S., KAMENETSKY, M.B., SOBOLEV, A.V., GOLOVIN, A.V., DEMOUCHY, S., FAURE, K., SHARYGIN, V.V. & KUZMIN, D.V. 2008. Olivine in the Udachnaya-East kimberlite (Yakutia, Russia): types, compositions and origins. Journal of Petrology, 49, 823-839. KOSTROVITSKY, S.I., MALKOVETS, V.G., VERICHEV, E.M., GARANIN, V.K. & SUVOROVA, L.V. 2004. Megacrysts from the Grib kimberlite pipe (Arkhangelsk Province, Russia). Lithos, 77, 511-523. KUKKONEN, I.T., KINNUNEN, K.A. & PELTONEN, P. 2003. Mantle xenoliths and thick lithosphere in the Fennoscandian shield. Physics and Chemistry of the Earth, 28, 349-360. LEHTONEN, M.L., O’BRIEN, H.E., PELTONEN, P., KUKKONEN, I.T., USTINOV, V. & VERZHAK, V. 2009. Mantle xenocrysts from the Arkhangelskaya kim- berlite (Lomonosov mine, NW Russia: Constraints on the composition and thermal state of the diamondiferous lithospheric mantle. Lithos, 112, 924-933. LEUNG, I.S. 1990. Silicon carbide cluster entrapped in a diamond from Fuxian, China. American Mineralogist, 75, 1110-1119. MCCLENAGHAN, M.B., 2005. Indicator mineral methods in mineral explo- ration. Geochemistry: Exploration, Environment, Analysis, 5, 233-245. NIXON, P.H. & HORNUNG, G. 1968. A new chromium garnet end member, knorringite, from kimberlite. The American Mineralogist, 59, 1833-1840. SHIRYAEV, A.A., GRIFFIN, W.L. & STOYANOV, E. 2011. Moissanite (SiC) from kimberlites: polytypes, trace elements, inclusions and speculations on ori- gin. Lithos, 122, 152-164. SPETSIUS, Z.V. 2004. Petrology of highly aluminous xenoliths from kimberlites of Yakutia. Lithos, 77, 525-538. STACHEL, T. & HARRIS, J.W. 2008. The origin of cratonic diamonds – con- straints from mineral inclusions. Ore Geology Reviews, 34, 5-32. Indicator minerals in diamond exploration: A case study from eastern Finnmark, Arkhangelsk and the Devonian Belt 12 Indicator Mineral Methods in Mineral Exploration, Workshop 3, 13-18. 25th International Applied Geochemistry Symposium Exploration for the RE and REE and other high-tech metals (Ga, Ge, In, Li, Nb, Ta, and Ti) is presently active in Finland. Also, the Geological Survey of Finland (GTK) has launched a four-year project (2009-2012) to investigate the country’s potential for high-tech metals. As a part of the project, soil geochemistry and indicator mineral methods have been used to trace potential sources for mineralized bedrock. Methodology used for the exploration high-tech metals is basically the same as for other commodities, such as base metals, gold, and PGE. Also, new methods have been developed and tested during the recent years. Till geochemistry is a key method for exploration in glaciated terrains. A regional till geochemical database and numerous target-scale datasets collected by GTK are the foun- dation for estimating the potential for different regions in Finland. Chemical analyses done using ICP-AES and/or ICP- MS methods include several elements applicable to high-tech metal potentiality estimations. For example, elevated concen- trations of La, Li, Sc, Ti and Y can be used for targeting stud- ies or for choosing samples for re-analysis with special meth- ods. New sampling and detailed fieldwork can be done using test pit surveys and percussion drillings. RE and REE anomalies in till exist only in ppb or ppm lev- els, but normally occurring as heavy minerals they can be con- centrated using gravity separation methods, such as the Knelson concentrator and heavy liquid. The minerals can be concentrated further by magnetic separation. The coarse fractions (>200 μm) can be investigated by hand picking under optical microscope. However, the microscopic identification of RE and REE minerals is challenging and requires a lot of man- ual SEM-EDS (scanning electron microscope + energy disper- sive spectrometer) work to analyze the selected individual grains for chemical composition. The searching for and analysis of the indicator minerals can be also automated by using a modern SEM and suitable soft- ware. One of the most exciting new applications is the fully automated study of the till fine fraction (<63 μm) mineralogy by the Mineral LiberationAnalyzer (MLA). The MLA consists of a modern FEI Quanta 600 SEM, two energy dispersive X- ray detectors, and JKTech quantitative mineralogy software, which allow quantitative analysis of mineral and material sam- ples (Fig. 1). The analyses are done from the monolayer pol- ished sections of the heavy mineral concentrates. In this paper, two case studies from different parts of Finland are presented to demonstrate the applicability of MLA to detect RE and REE minerals in soil. CASE STUDY 1: REVONKYLÄ AREA IN ILOMANTSI, EASTERN FINLAND In the Ilomantsi study area (Fig. 2), a pyrochlore anomaly had been discovered in till during an earlier heavy mineral survey for diamond indicator minerals (Lehtonen et al. 2009). Altogether approximately 100 pyrochlore grains were detected in the 0.25-1.0 mm fractions of three Knelson-concentrated originally 60 kg basal till samples. The grains were analyzed by a Cameca SX100 electron microprobe, and compositionally they could be classified into (1) yttro-betafite-(Y), (2) yttro- pyrochlore-(Y), and (3-4) uranobetafite varieties (Fig. 3). The source for the grains remains unknown. Based on the micro- analytical data, both pegmatitic and alkalic source rocks are possible. In the context of the GTK high-tech metals project, additional sampling was carried out in the area. The sample processing flow sheet is given in Figure 4. For the traditional indicator mineral work the samples were processed as in the previous study, using the standard Knelson- based protocol for diamond indicator minerals (Lehtonen et al. 2005). -63mm sample material was subjected to geochemical (ICP-AES, ICP-MS) and MLA analyses. For the MLA, the heavy mineral fractions were concentrated using HMS (heavy media separation) and LIMS (low-intensity magnetic separa- tion), followed by mounting in epoxy. The analyses were car- ried out on polished monolayer mounts, where graphite-pow- der was used to separate the grains. From each sample 2 to 4 mounts were made, corresponding roughly to 300,000 to 800,000 individual mineral grains. Energy-dispersive X-ray (EDX) analyses were taken from all heavy mineral grains with density higher than that of zircon (4.7). The selection was based on backscatter electron (BSE) imaging. Exploring RE and REE mineralization using indicator minerals M. Lehtonen1, J. Laukkanen2 & P. Sarala3 Geological Survey of Finland 1. P.O. Box 96, FI-02151 Espoo, Finland 2. Tutkijankatu 1, FI-83500 Outokumpu, Finland 3. P.O. Box 77, FI-96101 Rovaniemi, Finland E-mail jukka.laukkanen@gtk.fi Fig. 1. The Mineral Liberation Analyzer (MLA). Photo: Geological Survey of Finland. The results of geochemical analyses show no anomalous contents of RE and REE compared to the regional back- ground. The MLA analyses were carried out on those samples where pyrochlore grains had been found by hand picking of the coarser (0.25-0.5 mm) Knelson-concentrated heavy min- eral fractions, and samples taken adjacent to them. Pyrochlore was detected in all analyzed samples, 24 grains per sample in maximum (Table 1). The results correlate well with those by hand picking, the most enriched samples coincided by both methods. It can be also estimated, that the number of mineral grains studied by both methods was roughly in the same order of magnitude. In addition to pyrochlore, the MLA detected other REE- bearing minerals (columbite-tantalite, monazite, xenotime and allanite). Many of them were found in even higher concentra- tions than pyrochlore. By hand picking only monazite was detected, which was by far the most common REE-bearing mineral in the sample material. The absence of the other REE- minerals in the hand-picked concentrates can probably be explained by their difficult recognition under optical micro- scope. CASE STUDY 2: SAARISELKÄ-PORTTIPAHTA AREA IN CENTRAL LAPLAND In the other target selected for this paper, the Saariselkä- Porttipahta area (Fig. 5), samples collected for gold exploration had showed anomalously high concentrations of lantanides (e.g. yttrium and cerium) in till and weathered bedrock, when compared to the regional background. The aim was to find out into which minerals the lantanides are bound, and moreover, the reason for the geochemical anomaly on the northeast side of Porttipahta. During the exploration, only monazite grains 14 M. Lehtonen, J. Laukkanen & P. Sarala Fig. 2. The Revonkylä sampling area (1), Ilomantsi, Eastern Finland. The sampling sites are indicated by dots, the arrow shows the main ice-flow direction in the region. © National Land Survey of Finland licence no MML/VIR/TIPA/217/11. Fig. 3. The microanalyses of the Ilomantsi pyrochlore grains shown in the compositional classification diagram by Hogarth (1977). The numbers 1 to 4 correspond to (1) yttro-betafite-(Y), (2) yttro- pyrochlore-(Y), and (3-4) uranobetafite. 15 had been detected in the heavy mineral concentrates of the originally ~20 kg samples, but no other REE-bearing minerals had been found. However, in the mobile metal ion (MMI) studies conducted in the area there were clearly traces of ele- vated high-tech metal concentrations (Sarala et al. 2008). The remaining sample material from the Saariselkä- Porttipahta area was subjected to further investigation. The coarser fractions (0.25-1.0 mm) were concentrated by heavy liquid and studied under binocular microscope and SEM-EDS. The fine fractions (-63 μm) were analyzed by the MLA using the same procedure as for the Ilomantsi samples. From each sample 2 polished mounts were made, corresponding roughly to 300,000 to 400,000 mounted mineral grains. Interesting grains identified by the MLA were subsequently analyzed by a Cameca SX100 electron microprobe. No REE-bearing minerals were detected during micro- scopic work of the coarse fraction, but the MLA investigation revealed several of them (Table 2). The samples contained abundant monazite (max. 12,000 grains/sample) and another mineral (Fig. 6) close in composition to it (max. 20,000 Exploring RE and REE minalization using indicator minerals Till sample 60kg Knelson Concentrator Dry screen 0.25mm Grain size analysis Wet screen -63μm Bisection Geochemical analysis HMS d>3.3 LIMS Wet screen -63μm Bisection HMS d>3.3 LIMS Hand picking SEM/EDS EPMA 2 subsamples MLA analysis Wet screen -1mm LIMS Geochemical analysis +0.25mm -0.25mm HMS d>3.3 LIMS MLA analysis (á 2kg) Fig. 4. The processing flowsheet for the Ilomantsi till samples. LIMS = low-intensity magnetic separation, HMS = heavy media separation, SEM- EDS = scanning electron microscope + energy dispersive spectrometer, EPMA = electron probe micro analyzer, MLA = mineral liberation analyzer. 90hoP_U_62490seK_U_62490niP_U_62490hoP_U_1E62490niP_U_1E624RM71_U624RM01_U624RM60_U624 lareniM tnuoCniarGtnuoCniarGtnuoCniarGtnuoCniarGtnuoCniarGtnuoCniarGtnuoCniarGtnuoCniarG 422142113223)Y(-erolhcoryp-orttY 11serolhcoryp_rehtO 60157512etilatnat_etibmuloC dloG 11 htumsiB 1 etiyeldeH 13 4211123212etileehcS 529251032361149etirohT nocriZ *26861*82751 488221623etiyeleddaB 982171315363040279510656401656etizanoM 037211652361415etisantsaB 1856841301401655737emitoneX 72026211etinallA etilonocriZ 11 111etisomahC 00291779718234105226912764811157latoT mm0.1-52.0fognikcipdnaH 66008126600)Y(-erolhcoryp-orttY .tnemerusaemehtnidedulcnisawnocriZ-* Table 1. The MLA-results of the Ilomantsi heavy mineral concentrates, fraction -63 μm. grains/sample). This water-containing mineral is more enriched in Y and Nd and less enriched in Ce compared to monazite. The mineral was identified as rhabdophane based on microanalytical data. In addition to monazite and rhabdo- phane, xenotime was the third Y-bearing mineral in the sam- ples (max. 2000 grains/sample). When crosschecking
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