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(DAI.{M, V 1. 0; 09-87) panphfet,
xrr{Eeir. sEpaRA{,ToN TFa'tfNaorrEs (DAI.{M,V 1. 0; 09-87) r.hich ls based The so.7e enphasis of this panphfet, an the ',ainly but conplete, is to experience of the author and is everttxhinq give you an idea ,rhat night be done by nov and in vhich ,ray in our nev nineraL separation 7ab. since it is also ditected to the very tbeginnertt you night tind sone expianations or advices t&undant. The author in any case vouid deepiy appreciate any codnents suqqestions concerning the nethods describd and asks the to cLose his eyes on the af7 too obvious Languaqe nistakes. I. ot reader PREPARATIONOF SAI{PIAS Techniques used for rnineraL separation depend upgn the purpose of poorLy analysis and lrhether or not the sanple is unconsolidated, or, is a !'e1l Lithified or fairly consolidated, sedirnentary rock neight or a crystalline rock. sone projects requj.re deternining percentages of various and also an a sanple, exanination af the shapes and surface textures of ninerals. Other pure projects require the separation of clean? virtually concentrates of indivj.duaL uj.nerals for chenical analysi6 rdithout minerals in described reqard for nineral tlorphology. The beLov briefly operations are appllcable to sedinents as well as hard rocks, even so initiaL handting procedures Day dlffer. :l'+ a. UNCONSOTIDATEDoT WEAKLY CONSOLIDATED ROCKSI particles, grains First nust be cl,eaned of adhering fine-grained gand graj,ns such as clay coatings on feldspars. Beach and rlver put the Earple in a are usually fairly clean. After sieving, nater and place it in a sonic vibrator. The beaker of destilled particles, sonic vibrator scrubs individual cleaning then af adhering or finer-grained tf adhering laterial is an oxide is necessary. Fe-oxj-de coatings Hcl (1:5 H2O), but avoid prolonged Day be reDoved by dilute are present. Dilute acetic treatnent, especially if rnetasilicates acid (1:1 H2O) uj.ll generally dissolve carbonates. If the purpose do is to exanine the Dorpholoqy and surface narklngs on graing, not carbonate, daterial. leave chernical treatnent then in a sonic vibrator nore than 1',/.h to 2h or in acids too long! Partially consolidated rocks require additionaL operations before scrubbing in a sonic vibrator or acid treatnents: (not grinding! ) in a clean Break then by gentle crushing nortar and pestle, especially if shapes and surface textures are to be studied; screen the broken rock throuqh a 2nn gieve to eliuinate slrall particles that are broken by crushingt place the pea- aDd walnut-sized fragnents in a jar containing a steeL roller agenc and about a leaspoon of dlsperslng (e.9.: sodiuD hexanetaphosphate ) , fill the jar rrith nater and r o l l th e j a r fo r l h to 2h on a jar nill; - (6ave the lrash the sedinenC through a 60/r! (25onesh) -screen finer-grained Daterial for possible pipette anaLysis) t scrub the sand in a sonic vibrator cleaningt for further the sanple ls novJ ready for 61zing by sievlng and further oDeratl0ns. b. HARD ROCI(S (SEDIIIENTAR9 or inltl.al hard rocks rEqulres fron (or weight) of rock crushing, sieving and cleaning. The size needed for getting nineral Eeparates varies according to rock tltpe be enough for and the purpose of analysis. cenerally 5009 vilL special. fineto silicate However, nediun-grained rocks. Any separation CRySfALIINE): of ninerals populations U/Pb aeparation of, zircon for like deternlnatlon Dight requi.re sanple sizes in excess of 50okg. operatlons age Prelininary thin section exanination is hiqhly advisable to determine lhe approxinate percentage and grain slze of ninerals, in the rock sanples. Thls will belp to establish vhat nesh size(s) lhe sample is to be ground. The nesh-size needed for nineral separation depends on the grain size, inclusions, zoning and intergro\tths, The sample should be ground fine enough to release the particular nineral fron its inclusions or intergrowths. parCicular zones are to be separated in zoned ninerals, should be as fine as the zone widths. $aterial If the If ni.nerals are different in hardnesg or size in the sane speciDen, a prelininary concentration can be done during grinding. In a garnet-chlorlte schist, for exanple, the garnet will be concentrated in the coarse fraction and the chlorite in the fine. In granitic rocks, the accessories often occur in the <l8o,.n ( < 8 o r n esh-fra ) cti o n . Ms furthemore inportant to work with a uniforn-sized satople in nineral separations because the techniques described bel-ord depend on physical properties or forces for separation. These properties do no! react unifornly vith naterial of unequal size, particularly Eagnetic separations where the same nineral of different be preferentially separated by nagnetic attraction. Crushed DateriaL is best partj.cul.arly contanination, solder water and netal afler frag[ents. size nay si.zed by sieving, but gRrard against lrith brass gieveg ehich nay introduce sieves should b6 nashed with desti].led each operation to renove in the adhering fragments (or llesh. Disposable PTrE sieve nets hel-d in cuC PP bottles wharever acetone-resistant is at hand!) is a nore satisfactory is nethod of sieving because little or no contaDination introduced. Renove all the fine particles once the required neshthe nineral size is attained. This nay be done by elutriating grains in aqua dest. /ethanol/nethanol or acetone or gcrubbing then for th to 2h in a sonic vibrator. Many rocks nineraL contain separations. alteration rron oxide products lrith the interfere and carbonates nay inpregnate or lrhich surrounal the nineral grains. this undesirable naterial prepared gallples are ready for II. Gentle acid (aee earlier IIAGNEAIC SEPARATIoN treatlent uill further dlscussion! ) . operatl0ns. (fRANlz ISODINAIIIC reDove The so SEPARAIOR) INTRODUCAION: The Frantz separator is excallent concentrates of thould be taken in its use centrifugo separates froD analytical lrork. extrenely vergatile and can produce nany Dinerals. soDe caution Iloirever, and in Dost casea, the Frantz beforE It Day be furbherDore suggested parphlet read this carefully, frustration. to as the it user, niII it is advisable they arg u6€d to for to take the tiDe save hiD delay and and FIJNDAUENIAI,S : property uagnetic susceptibility is an iDportant of toinerals. l{inerals are paralragDetic nhen nagnetic force Iines pasE through them lore easiLy than lhrough air, and are diaDagnetlc when they paas readily. g.n.ral Beaides this description, thsrc are six different t)Tres of Dagnetic naterials (feel free to skip thig over! ) : OIAII'GIIETIC:TI€SE UTdIIi I'IICH THEIIA6TTIC II{OIf,IIOI IS SLIGIITLT LESSTHAIITNTAPPLIMMGilETICFITLOi olurcx€Tlsrts lti aro{c scA.tcorisEouEtlcE 0FTHE LENz-uc 0Flliolf,Tlor t m olfl GlEltcnTaIlLs, THtPIO{EILITYlS SLIGIjTLY ttSSI}l^Xth T 0€ Eft?Tt splcE, AltDTltEtt EitTlcsuSCtpllElLtTY IS iE6Tltt lio sr LL. PARAIiAGiETIC: TIiOSI |lTHIIi VIIICIjTHEIAGIITTICIIit)lJcIIOIiIS SLIOIILYGREITER THAI{IhE APPLIOI{IGITIIC FIEIO; PATIIAGIIETISII TTISESFNOilHT PARTIA!A!IGI{4EIiT I{ATflIC OIPOLE IOIEIiIS Of AIOiS OT OF Iffi P€NMNEI(T IOiS; THTPMTf|8II.ITI IS SLIOHILI TEAIENIHANTMI OF EIIPT'ISPACE, A'iD IIT I.IA6Ii€TIC SUSCEPTIBILITY I S P o S IT Ml r0 S XL L , FlRiotl6ltTlc: Trfst Iri $ cll TtiE NltNE c iqlEiTs 0F AT0ts 0N IoNS lli A t{a6[tTlc DfiaIi TEIiDIo Et aLl6tEo PATALLEL IO OIT IIIOTIITIII ZEROAPPLII! FITII), STLOtiI CHAIIITERISTIC IAIPERIIURE, CAI.LED TNECURIE P0I[i corPtErEoRDERIIG Is lcrlEvto oitt rT THt A8sorultrtm 0F rolPnrrnEt ylntr A ll^ filc Dfl lli, ATISSoLUTE IIoil 15 EQUAL I0 Tllt SlJr0F lrlE ll 6|{EIICrOrErlIS ZERo, THtiAGTiETIZ 0F Ttlt A]olis0R I0N5PtRltilT voLltlE taTTER,Corstsltm0f iaNYsHALL ilGt{ETIcmulis, hAsa ltETtt4qErlzaTlotl i BU|'"K (HySIER€SIS $tIcN DEPflioS UPoiTHEillGXtTtCHlSToRr 0F Tfl€SPECIiOT tFFtCr)i ttt PtFr€lEtLITIDIPI|OS 0x rHt t|^G|6ncFttLo, rxo ctri Rtlcr vatuts oF rHE0R0ER 0F 1OE+06 rlriEs Tlt T oF Fttt sptcEi a80vETrlEonlt P0lriT, THEst{aTERIAL BECCTE PAIANA6TIEIIC. AX]IFERROIAGilETIC: THOSE IIi iiIIICHTHEIAGNEIIC IONEIiTS OFA,IOI'IS ORIoIIs TEII|).IoASSL}4T AI{oROERE|) iRTAIIGI,IEIIT IIi ITROAPPLIED fIELD, slf,tJIIIAI TIITVECIMSWOFThEI{)IIEIITS I5 ZEiO. EEIOJ A CIARACTERISIIC TEIIPTI^TIJRE $!LED NE NEiL POII{T; ThEPTRIiT8III'IY NATERIALS OF I5 COIPARA6LT IO TIIATOF p MraorETIcrurtttaLsi ABow rHE NEiL ibltT,^|iTIFERNO|iIGIiETIC rHEst r TE lt-s BEcuiEpat,| 6xE ct eIttpLE3 HtlrTtTt. FERnl|ilGlltTlC: rO AsSUll€ TIOSEIrl ttlICUTtiEr,lG|iEIICrOlElTSOFAT0|SORIOIISTEIIO All OROERED 8ln rioll-PlllLLtL AiRAIGO,ITIIT III ZERO APPLIEO FIELO, EELOI NEE1t,OIiI; Ii THEUSUAL CASE, VITIiIIIA iTGrcTIC 'HE FRorTd€axrr-PARALtEL otli ri, a sr.BsrAtTIAL |lAGttTIzTlori RtguLTS arlcrartlll 0f ri€lclrsRlrGnri'rtT IHE EqUIvALErlt S|ELAITICE5. |,|ICR0SC0PIC IS T0 THII 0F FERROIIGIIETI Sl , A80VtTllE EEIIAVIoUR SIIIILAR i NErLPolfi, fitsE taltRl^Ls SEcottpaR{u6iETIc. riETrt ErtTlc: TrosEsllch FEtfln EiEIIc Il{ ttlt FItLos, Bw nitclt lEcotEFENR0roElErlruLy soEtlD ]n ^iE ^ri S1ROI6 APPLITD FITOS. Conlron paralagnetic nlnerals are dioptase; pyrlte, larkaglte, dololite, !.Emeaite, beryll, coNlon dl.aDagnetic subgtances are: copper, gold, silver, galena, quartz, lead, sulphu!, halite, calqlte, f,luorite, tolra8, zircon (only if very pure!) i the following ferroragDetic €I€!€nts: avaruito: l(nown group: terreEtrial ninerals belong rutile, blsDutb, alEtlt€, the Fe. Co, Nl, Gd Nl'Fe (crystal lattice of Ni, ca. 78* Nir connon in serpentlnltes, e.g. Josephine Co., OR, Ararua. New Zealand) t vairauite: CoFe (coruon In Eerpentinites, N e w ze a l a n d) ; lagnetite: F e --F e rr!.o ., lagmoferrite: ja*obsite: ltgFezO. t HnFe'o. (in lIlrestones; heavily nagnetic!); (narbles and skarns, (zn, Un':) (Ferrr, Hn!r!)iO. frantlinite: e.g.: wairau vaLley. e .g .: trevoritei lagheDite: cubanite: Prrrhotite: F ra n k lin, NJ) t NiFe2o. (rare, e.g,i Barberton, Transvaal) from nagnetite, \didespread, e-Fe.o" (originate e .g .: Iro n ut., Shasta Co., CA, Bushveld, Transvaal, Sierra Mutun, Bollvia) cuFe"s. (vlde6pread, e.g.: uorro ve1ho, Bra6l,l, NaDibla, Ellanar-Distrj.ct, Alaska, otjosongati, Kaveltorp & I\rnaberg, Sweden) t Fes (only Eonoclinal 4c-phase!, videspread, (Ni, Fe)'S., espeqlally associated with pentlandite nore rare: in Dafic rocks (gabbros/diorites, basaltoidE), dykes in pegiDatltlc-pneulatol)rtj.c (e.9.: Tysfjord, Norvay, Tunaberg, sweden), ln dykes (e.g.: Morro velho, Brasil), both. contactDetanorphic aureoles and (e. 9. : Bajuvarian regionalnetaDorphic terraines hydrothernal Forest, w-Gernany, CSSR, Ducktosn, the Baltic Shield), in sedinentary e .g .: C ri tnea, USSR) . In nineral separation we uEe the TN, coDDon to rocks (rare, (s), Eas8-susceptibifity ELven byl 9 tz s = l t(P -L l / ( 4n9r ) I E+o6) ; [cn' g- ' ] specific density of a ninerali nagnetic pemeability of a nineral. Dagnetic dinerals: nomally nagnetic Dinerals: veakly nagmetic uinerals: non-lagnetic ninerals: heavily s = s = s = S = (1 ) 3 5 , O 0 0 E+O6 cD'g-a; 3 5 , 0 o o E+O6 200 in cD'g-!; E+06 cn.g-a t < 2 0 0 E+O5 cn.g-1. rdhiqh 16 In general Cenns, the grouplng of either ferro-, a nineral nill para- or dianagnetic elenents in the structure of lnfluence perDeabj,Iily. since elenents of al,1 six different Dagnetic its vi11 not neceEsarj.Ly be types nay be present, a given nineral para-, either diaor ferronagnetic. Para- and ferronagnetic ninerals are attracted lrhen placed in a nagnetic field, a property Frantz isodynanic separator. This property is IesE chenical variations than is density, but bxtrenely clean separations can be nade only \rith certaj.n nineral.s. used by the sensitlve to is only possible applying an inhonogeneous, isodynanic fieLd, where translatory forces are produced. In a hodoqeneous field the inserted are only affected ninerals by a parallel nonent of rotation and subsequently oriented to ehe direction r,ithout of the nagnetic field, any further novenent. A field is called isodynanlc, if at any given point the product of (/o) , field-strength (H) and the change of the induction-constant A nagnetic separation (grad H) at a gj.ven point of the vector-field fieldstrenght (on the direction norr0aL to lhe equipotential-planes decreasing H-values) equals constant: ( 2) gr ad H = const ,/Jo *fl + 3. in the side of GENERAIJREMARKSON THE FRANTZ ISODYNA}IIC SEPARATOR: The separator consiscs of an el,ectrolagnet vith a slot betrreen its pole shoes. A chute made of non-nagnetic naterial is nounted in this slot which can be set vibratillg at an controllable anpliUud6. The whole nagnetic systeh can be noved around two axeg, vhereby the direction at right angles co the length of the chute will be qalled side slope, and parallel to the length, forr,ard alope. The Dinerals to be seperated are inserled the into systelo by Deans of a funnel. The shape of the pole shoes is calculated Therefore the naqmetic force F- effecting to fulfill a nineral equation (2). graln is given by: (3) Fi=CrX*12rV I: exciter anperagei C3 constantt x: Eusceptibility t v: volune of nineral grain. The side 6lope P resuLts in a gravity Gr=y*vi9r co6p g : w e i g ht o f th e u i n e ra l gr ain; . ^^- r , , ^+ conponent cl ( 4) 1 ., i + ,,, directed opposite to the lragnetic force. If cr>F-, the nineral gra1ns nove to the lover side of the chute, if c"<F- the resulting novenent is directed vice versa. At a given side slope F and g.ains exciter aDperage the clas3ificatlon of lineral along the chute is deperdent onLy upon their specific susceptibilityl A! j.ts Iover end the chute is dtvided by a center rail, so two different susceptibility classes can be extracted into tvo beakers. By systeoatic change of ttre erciter a lixture arperag€, grains of different lineral ca! be Eplit into different Eugcelrtibility-claases ! ThereforE lhe nost lDportant aettings Ere Eid€ glolre .l, and exciter a4rerage ! Both, fortrard slope and vibratl,on aDplitude define only the transport velocity within the chute and the tine of separatlon respectively. SOIi{EI!.{PORTANTFACTS BEFOREGETTING STARTED: a, Itnder all lhen fror the aeparator carrylng a CARDIAC-PACEI(AXm.- othen ise thls night have been the last \rork you tri.ed to perforol You also night not rrant to carry a hearing-aid, since interference of this device generated lrith the strong electroEagnetic flel,d by the separator clrsulstances, night Etay avay cause severe daDage to your inner ear! 9 b. Do not carry a natch - this night cause the sudden rrdeathrr of jelreL or at least your precious vill not be very rduch appreciated by its electronics! AIso, remenber: You are dealing not with rant a very to strong use electromagnet: screrrdrivers, close to the pole sililar tools just as fast as strongly You therefore pocketknifes spatulas, shoes - because those vill do or be attracted by the nagnet! IN.'I'RIES OR DA!{AGETO EOUIPT{ENT ! --------------AVOID c. Make repeatedly sure that the funnel is scre!,/ed in tighbly and noC becane loose by the osciLlati.on of the chute! Do not overfill the funnel very fine-grained llaterials - since behave alnost d. uake sure e. Reuove all f. g. like Newtonian fl.uids, they tend to spj-Il! ahead of any separation that no ferroDagnetic or paraDagnetic to the strongly lateriaLs are left clinging chute or pole shoes. You oight l{ant to clean the rather (using a fine paint-brush! ) again, apparatus of instead spoiling your aarnple! (abraslve ferroDaqmetic Dinerals and particles grinding!) crushing, loading the saDple frou forner before (using into the separator the nethod described further positively below!). Even very few of those particles will clsan-up block the chute and vill lead to spi1l, requiring and to repeat the separation (think of your precious tine!), and Dight even cause loss of your saDple! uake sure your sanples are not contaninated vith dust, Ij.nts or overslzed nineral grains! Dust causes static charge, lints and oversized grains blockage of the funnel - both lrorsen seriously the results of your separation! Do not leave the separator unattended or let it run uithout load! The effecliveness of your work is highly dependenc upon continouity the - i.e. the quality if separation you stay vill be achieved nost in separator uhile vith the highest runnlng and add naterial constantl.y! Renehber: The throughput of your sanple is not only dependent upon forward slope and anperage, but al-so content of higher exciter upon paranagnetic ninerals! l0 Nornally a side slope of approxinately 20- is used and a forerard slope near 3Oo. A steeper forrard slope nay cauge the graj.ns to bounce rrhen coarser graj.n sizes are being separated nhereas too snall a slope with finer grain sizes lrili inpede free flov of the sanple down the chute. Snaller Eide slopes (2o - 10o) are used t'o separate the Dinerals irith very snall nagnetic susceptibil ities uhich lrould separate on the nonrnagnetic side of the chute at a 20- slope and Daxinun current. Hovever, vhile standard settings of 20- side slope and 30- forrrard slope are norhally used, these val,ues are not at aII critical. Uany laboralories use 10- to 15- 6Lde slopes and snaller forward slopes. So any satj.sfactory aetting can rtrial easily be deten0ined by & errorrr - feeL encouraged to on your own settings! Rate of flow is controlled by screwing the input funnel up or doun. SiDilarl-y a steeper forrrard slope eill increase rate of florr or a qentLer slope decrease it. The proper rate of flol, can be judged by eye after a little practice. U6ualLy, given try the slopes suggested, a flov rate of +/-lcn.Din-' will result, However, rapid initial separatlons such as the renoval of 90* quartz + feLdspar from a rock in nhich it is desired to concentrate present a nagnetic in 6DalI nineraL aDount, can be nade at +,/-5c[3nin-1. a rate of Final purificatj.on of the desired nineral lrould than be nade at perhaps powders O.3cn.nin-l. But you should rerneDber that fine will flow at sonetthat lo\der rates and coarser at faster. The thickness of the strean of povder should be kept aliJayg the saDe. Once having observed the proper strean thi.ckness, there is no difficulty in adjusting lhe flow for any grain size or slope to conforE to this optlDuD strean thickness. In qeneral the ganple should be at least roughly sized. Ordinarj.Iy Eeparations are nade in the range 63F! - 18O|u (DIN 4f88), or 23oDesh - 8oresh (AsTu E11-7o) respectively. 50qp! (3oDeah) is about the largest sj.ze on vhich geparations are convenient and 45,F8 (325Desh) about the snallest. With the finer difficulties nay be encountered fron eLectrostatic charge on the particles and consequent "balling upn. If, however, the sanple can be disaggregated, good separations can be nade dovn to 4 5ptI or 325nesh respectively. k. Do not sizes forget to CLEA}| the rhole apparatus as vell as your operation eveything else used during I{EDIATELy after uee! That prevents not only spoil.j.ng your samples bue will be greatly appreciated by the next user! For cleaning of the nagmet, especially the pol,e shoes and the preferably. chute, use carbon tetrachloride It is j.nportant that no OIIJ or any cleaning rnateriat containing GRAESEshoul-d be used under any circudstances on these partg, since even a thin filn of oi1/grrease viII cause qrains to etick and either lnpair l. 4. ---A. the separation or cause cutting of the sliding parts. Report al.l accidents or datnage to equipnent innediately - so it can be Caken care ofl HOW TO USE THE FRANTZ ISODYNAI,IIC SEPARATOR (ALWAYSSTART WITH A. BEFORE PROCEEDINGTO ANY OTHER STEP!)--- Preparation of salples: Use the binocular first to compounds in your sanple i prepare a fraction betveen find out about qrain 63Fn and 18orrtn or (for restrictions sieving Eizes and 23Otnesh to an grain Sonesh respectiveLy, by si.zes see abovel ) t lrash your Biewed satnplo using ethanol/hethanol or acetonei do not use destilled vater to avoid staining of the grains by iron oxide produced froh iron filings; this nay t0ost easily be done by stirrlng the sanple in a beaker of solvent, alloving to Eettle it for 2Os and decanling the solvent several tines, or by scrubbing j.t in an ultrasonic cleaDeri (wash and dry in proper ventilated hood only! Do not use infrared separation la[ps in nineral Lab to dry sa.qrles previoqsly rashed ritb organic solvents ! ) t dry sanples; saDples d. use binocular again - if still heavily contaninated irith dust ( reDenber: grains or Linls If lhe are dust-coated, the quality of the separation nay be Eaterially reduced!): Repeat step c. (decide vhich type of ninerals you need to separate and for vhat purpose: You Dight fi,nd it suitable to use diluted acj,ds (HNo", HCI) for further cleaning, If you do so, you have to wash the sarnple several times using aqua dest. afterwardsl Rehernber: Thig night result in Etaining, so you night find it worlh to renove iron fillngs nith a paper- e. vrapped hand-nagnet firstl)t if only fev contaninants renain, use hand-picking for final clean-up; try to uake sure that naxj.nu! grain size is snaller than particles intergroltn extract intergroi.bhs by - otherwise qrain sizes or sieving using finer either nilling to finer maxinun sieve-size. and d. ! B. you had to go through this, repeat c, particles fast Eeparation of ferroDagtretic and contalinants: Take chute out of pole shoest (using turn both hands) nagnet so direction of slot is vertical i cover whole length of slot with paper and fix it to the pole shoes using Scotchn (or lrhatever else suitable) - DO NOT (thiE LEAVE ANY PART OF lHE POLE SHOES UNCOVERED! I! positively lrill put a wide Renenber, in a lot of trouble for you!) t ( 0.1 exciter anperage A i6 definitely result s!.itch on lor sufficientl ); e. If porcelain/glass/aluDinuD you are dealing with (NO a naqnet...) STEEL beaker PTEASE!! ! underneath the end of lhe slott or build yourseLf a funnel using ghick aluninun/plastic foil paper and for! the outlet 9o it t0atches the shape of the slot (you night as vell use a plastic funnel for Dore pernanent usei to ho{ever, avoid cross-contanination of different sanples, you better build a ne!, one every tine!) t !t. let the sanple faLL into the beaker; freely and at good pace through the sLot particles RESULT: Ferronagnetic paper, Eo the or contaEinants gtick to the sanple wiII be freed of then alDost quantj.tatively at the first run. h. Take another beaker - switch off anperage and all this stuff is 9oin9 to fall into this beaker. ferronagnetic (it happened to ne several SUGGESTION:Do not hix up beakers.... linesl). Repeat this procedure at least ttro nore tilres to yield good results; if you feel you already dj.d a good job on and 'ran)rnay you are short of tine..." not having followed this advice, but will as I was first doing thisl) not to skip it that ---CIJAN - you night regret be convinced (saDe the next tinel THE FRANTZCOI.{PLETELY ! ---- C. Fast aeparation a, b. Take the chute out of the s1o!t adjust foroard slope to about 85-, side slope to about 2--5-; insert funnel. (see abovel) inlo slot facing tolrard yout design a nsample-separatlng devicert (carton, cardboard) and c. d, of dia[agnetic Dinerals: e, nount to Lolrer end of slott provide tlro beakers underneath carton; e. slritch on high exciter f. insert saupl-e like RISUI"TI only stralght to you) . outlet anperage (at least separated by this 1..2 A)t during B. grains wiIl, not be deflected and fall dianagnetic downuards into the provided beaker (the one closer qrains and suitch off Dagnet Renove beaker lrith dianagnetic all. paraDagnetic graj.ns irill no!, fall into beaker left, SUGGESTIONS:Buitd "sanple-separating-devicel in a nanner, that rrseparating you are able to insert a nallir about lrr into S. Repeat this procedure several w i t h yo u r b e a ke rs..... s1ot. ADVANTAGE: This separation sanple voLumes (up to anounts of is hj.ghly 2okg/day) dianagnetic ninerals tiDes - and do not Dix up greater reco!$ended for qreat of rocks containing quartz, feldspars, like 14 quartzites, e.g.: sandstones, IiDestones, nables etc. ! -------CLEAN THE FRANTZ COT'{PLETELY calcj.te aplites, D. Reuoval of a[ounts of amounts sDall paraEagnetic b. ad just forward slope facingt for! ards (instead c. hang both d. adjust exciter e. insert sarnple through RESULT: flow rear separation 2' - 3- rate of chute; 1.2 A; rnounted to funnel lriIl paranagnetic chute, up be or adjust down, col.lected ninerals L'iIl. purifi.cation in look the for beaker into be deflected a especially (oDphacite!) for biotite-, pre-concentrates. ! ---THE FRANTZ COI,IPLETELY nineral mixture nDagnetictr into and 'non- fractions: side slope to (facing 10- backvards!), slope foryard 2 0-; c. set d. Lnsert exciter anperage to approx|nateLy completely'rseparaterr siritch off bin ocular all oscillation - there ninerals there and are chute; 0.1A; of 1cr[' sanple into funnel both fractions and Iet ; ahd vieu present are to find no separation in both taken species separates separation yielded under p o s s ib ilit ie s : sone )nineral non-magnetic quantitative of are t h re e has been virtually 2. least to s p illin g ; rninerals choose nediurn oscill.ation 1. at pre v e n t b. e. huge as usual:); hooks at end of into input provides of Dagnetic' to s id e of backvards the ---CLEAN Adjust s lo p e - funnel pyroxene- a.Dphibole-, a. 3 o -, frou beaker. ADVANTAGES: t{ethod E. 2o- beakers rate, you, to to anperage to Dianagnetic facinq the aluninuli screnj.ng constant ninerals in place; Leave chute by diaDagmetic veins, grains: a. flol, of quartz respectively place; - there place; enriched has taken beakers in the - nagnetic but no 3. In the naqnetic fraction consj.sts of one or nore nineral species, lrhich do not occur in lhe non-nagnetic fraction an).rDore - conplete separatj.on uas achieved. cases l. and 2. return bottr fractions to funnel ln case 3. only non-lagmetic f. fraction; anperage glightly: lncrease exciter c ase 1 .: a p p r, 0 .0 5 A; c ase 2 .: a p p r. 0 .1 4 ; c a se 3 .: a p p r. 0 .2 A t slritch oscillation of chute on; proceed vith your sauple has been separated step d. until into as Dary fractions obCaina.ble by this Dethod. RESULT: This is the most conplete separagion possible using the Frantz isodynanic separatorl !---------CLEAN THE FRANTZCOMPLETELY 5. GENER,ALCOUMENTS: Even so the Frantz separating ninerals having fairly sinilar careful variation of will isodynanic one night often susceptibilities. both experience of plutonic ninerals susceptibilities has is a polrerful diaBagnetic aDperage result. shown rocks sufficient that especially often slorrly cooled a gcatter in do not exhibit using llonever, for this Eethod. and vol.canic rocks generally displ,ay far have yielded rnineral.s : studies in nineraL species case even the nost Detanorphic, sedinentary greater variation and thus are nore apt for applying Enpirical tool encounter In this fl.ow rate and exciter slopes, not Iead to a satisfying Previous separator the fol-Lowing table the Franlz. for para- and 16 a. uagnetic fraction ollvine chrolite at slde alope 2O-l 0 .9 A: I.2 A: hornblende diopaidq hlDersthone trerollte auglte enstattte aktinollte spinel chlorltold heDatite staurollte epidote 0 . 4 A: ilDenite garnet biotite chlorite nschorln b. lld€ alope: 56r alpcrage 1.2 A: Dagmetic fractLon: non-EagnelLc fractlgn: titanlte zircon leucoxene rutlle apatlte anatalre andalusite brooklte nonaztte pyrite Xsnotine CorunduD topaz lluorlte kyanite silliDanlte anhydrite beryI dla[and Du3covlte zolglte clinozolsit€ turDallne L7 III. I. TIIE USE OF EEAVY LIQUIDS INTRODUCTIONI grains according to their of nineral The separation of nixtures specific density using "heavy liquids'r haB been used since alnost a 1oo years. Density ls one of the host sensitive Properties that up to about separations. Oensities can be utiLized in lrineral generaL the In !'ith beavy liquids. 5gcn-3 can be obtained Houever, frastionation. separation is rnade by a islnk-floatn nineraLs vilh densitites or jigging - techniques renove the l lghter 5gcn-3 nay be separated which use uater and eccentric over by Panning notions to fractions. the heavy sonte introductory renarks shoul.d also be nade regarding in you may use: IGUUBEIN & PETTI,TOHNsuggested already liquids, to should have the folloving attributes 1938 that a heavy liguid (i) inexpensive, (ii) easily prepared or purchased' be effective: (v) non(iii) (iv) liquid at ordinary te[peratures, transparent, (vii) tovards Dost r0inerals, inert (lx) easily diluted and not viscous, add - (x) non-Coxic. However, none of but soDe the heavy liquids now ln use have all of these qualitles, there is a tendency of the than others. f'urthennore, are better proporgional to their being directLy expense of the Liquids bc noted further density. 9o, in any case, and besides what !,ill down, all efforts should be nade not only to gain the highest (vi) corrosive, chenically odor, (viii) fluitl, vithout recovered, and - one should quality for of re-use. separatj.on of your sample, but to recover the liquids 2. FUNDAI.IENTAIS: Specifj.c density is a characteristic property of every solid or fluid at given pressure and tenperature. Using heavy liquids to separate different Einerals according to their speclfic density, the settling g: . gravity rate in a Nentonian liquid is given by STOKETSla!r: v = [2 sr2 ( 9c - gL) l/( etll ( 5) acceLeration; r: radiug of a spherical crystal 9- ,9-3 density of the crystal and the liquid viscosity Ti The density of Dinerals, several reasons: a. b. c. d. e. honever, by far the najority solutions, so their bight respectiveLy be widely variable due to of rock-forning ninerals are soLidconpositions night be lridely variable mixtures of up to four najor conponentsi specific lattice conponenls night be substituted by heavier or lighter ones; part of the hydrous phases nigbt be reDoved froE crygtal latticet ninerals Eight fluid/gageous separated; exhibit intergrowth inclusions lrhich with due other to size ninerals or cannot be ninerals containing U and/or Th night shov a tendency to isotropisation and thus decrease in density; the speclflc density of these Dinerals (e.g.: zircon, nonazite) can vary fairly ridcly. Density follolring ranges table of the tnost connon minerals (TROEGER,197t ) : are given in the 19 Densitiles the host corftron ninerals (except salts): 27 -0 lll4;!, ';3 zn-' laT t2/ 227 'l,tt 22! 2JZ 22tt zlz i tt z! lht tl/ ulz Jlu/Jort tttto/o ,run4r4/tt!t/4 I E/ :i It,t.) ,tt zaz /u'|'Jii/b !t4t41i E -l 612 nt / tza !!JhrJ2toun// A,aJ2/4 Jlulpt? qttp,tDl Ttrszaot L t! tE A4rptf !/Nvy a/n {4aa i -r q/ z! /t oz 0, 6 2r J? J .: Jit :110 JlJ Jt, t, @!',a,"'"",, ,',3 -- oan/l :tat ls tt,7?t /x/. /at ;"./ '1..)',.',,r""r lou f'aaarq r a nn/ntbi/t ij; /70 /7, Jr! L t J,;,' 1; 1'5 t? 22 density of a particular nineral - is the grain size of the sanple: Denaity separation using heavy liquids is virlually not possible for grain sizes <36 D (<4ooDesh) - unless one uses a centrifugel Iitost critical - besides that can just be estinated The fine uaterial dorrn sone lighCs SiDilarly, the has a tendency and the the lights sanple actual to clot with lhe heavies dragging lrill occlude sone of the heavieg, volune reconDended - given the ninirnum apparatus used - should not fall belou lcn.. On the other hand, it is possible to fractionate nineraLs having a difference in density of only E-02 gcm-5 - even so this requires painstaking ,ork. HEAVY LIQUIDS COMUONLY USED: s6.ri rrhh.|rvtuhgr.ltat., contains [3Na.WO..9WO..H2O], non-toxic, about 85.66* wo. and is readily soluble in water (up to 80 nass-* at 25-C; nass-* = {gram I substance ] /gram [substance + vaterl lrr100) . The naxir0un density of an aequous Napolytungstate (25-C), solution but can be is 3.12gcn-' extended by adding tungsten carbide powder to the saturated 6o1ution. of this cloudy suspension lrill than The desity reach up to 4.6gcn-3 (25o) by introduci.ng up !o 40& tunEsten stable lrlthin carbide. The aequous solulions are colourless, a pH-range of 2-L4 and are both, easy to prepare and regeneraEe. ptease For preparation and use of Na-polytungstate solutions, note the - foLlouiDq: vatert use only destj.lled uEie onLy glass containers; if poasible, contact sith do not the solution alloe to core into reducing agents. Horrever, if it should, tbe blue colour has no infl,uence on the density resultinq choseni pollrtungstate the vashing sol.ution particles respective evaporating pol)rtungstate to should vith the desired respestively. uashing ! be recovered aqua dest. density, Ilo not or use by and then addlng soljd any organic solventa for the garple Daterial to be separated should be free of soLuble Ca-coDponents! Othervise, Cainsoluble polltungstate vill be forled. A respective exanple are pleage eagh sanple clay Dinerals; if in any doubt, thoroughly in hot destilled water! tvo lajor the - disadvantages have to be relarked: viscosity of a Na-pollrtungstate solution increases very rapidly above a density of 2.59c[-3; tfa-poltrbungstate has a rather high trace el.euent (Xo: +/-2ppu; content As: +/-5pIrD: U: +/-lofrtD) that Dight interfere with chenical anal.ysis of the concentrates if they are not cleaned carefully vith aqua dest. to reDove any residue. For preparing golutions the follolring values are given for reference: desired density of heavy I iquid ( gcn - 3): Na-polytungstate to addi g (Na-polytungstate) nass-t ! 1, 0000!ol aq. dest b. 3.0 80. 00 77 .50 2.5 75.00 70.00 Bro[ofoEt, sensitive containing ICHBr'], to I j.ght copper naxinurn ( should filings density: be or stored nesh), 4,000.00 3,450.00 3,210.00 3,000.00 2,300.00 2.8949cn- ! in anber letabolic aC 2O- C , bottles poison, 25 inhalation flow of of tears exposure dahage c. sball and saliva, causes the amounts causes reddening lacriDation liver of and and cause provoking irritation, the face, nore narcosis, can the serious seriously death. (acetylentetrabromj.de, Tetrabronethan Muthnannrs solution), 2 . 9 6 ' 1 g c -3 a t 2 0 -C, s e n s i t i v e [C gB r=.CHB r=], naximum d e n s it y : (should be stored in ahber to light bottles containing copper fi.lings or nesh! ) , cancerogene. (dij.odonethan), Uethylene iodide 3.3259cn-3 arnber at 20-C, bottfes products and cause conjunctival of 20-C, toxic highly Rohrbach I s 20-C, highly Clerici and assimilated an lethal!), it is Tl nephritis, causes CIJRICI the reseDbles skin neight its degeneration density 3.1559cn-. of of bariurn 3 . 4 8 59 c n - 3 thal1i-uh such such a forltr body formate it rjith as ert thenas and in loss paralysis, of through and the skin noted from digestive above - Cleri-ci irill that hair, diaEhea, death, clerici and rashes; BE CONSIDERED THE T{OST DANGEROUS OF AI,L solution be [7D1 considered aokg! I are properties toxic causes can l'eight of and ultiDately in synptons in libbs coDpounds toxic potassiu![ solution intoxication tIQUIDS ! Thalliun the opacity of solution (O.49/kq body Pb in irritations ITIGIII is the cardiac blepharitis, of n ax i n u h I 1 1 2 c a H2 0 4 ] , 5 . I o g c n -3 / 1 00 - C , 4 . 6 o g c n -3 / 9 O -Ci poison, in absence rn a lo n a t e average pains craDps, the overexposure; solution thalliurn a cuhulative heshl ) , nervous h a x irn u m d e n s it y I B a (Hg J " )] , nercury coBpound; thalliu n into considering frod equirnolare because edena, aequous 4.O4gc1\-3 / 2 O -Ci poisonous ttle aequous toxic solution, ITlHco2] de nsities: vision, effects solution, te traiodomercurate-II at of [K2 (HgJ") ], maxinun Dercury conpound; iodohercurate-I1 or dardage pulnonary reflexes, filings seriously derangement cornea and fatal Thoulet I s solution, at copper can the tetra to containing deconposition systeD s e n s it iv e naxirnum density tCH2I2l, L j. g h t (s h o u ld b e s t o red in are readily tract cause absorbed causing alnost HEAVY the instant lrhite (Iater coloration silvery-grey! turning ) on contact lrith into shiny, Detallic the skin. General remarks: With the exception of the pollrtungstate, Thouletrs-, of described the above properly ventilated PROHIBITED IN the use organic heavlt provided rrith person safety precautions. - aLways clerici; skin, with even - eatinq,/drinling (see or Iaboratory and near clean t!!e area after use - these the BASED dispose off solvents in report ON CHEUICAI,S ABOVE of uhat all STATED DEFINITELY DEFINITELY This also vapors hood has of to be adequate of physician detergent; left the alL next to you bight so, in y o u r e.g. for above r.atch in the prohibited; apparatus iuEediately not shat he no6t knos, likely eill tteavlr liquids you not be g la s s n a re . . . . . ; positively - your solutions; positiveLy and - vith lunches/beverages is r.ith iDDediately if reaction already be trenoughn.-.!); in with, sorking contact sorked user is take nhile slightest lots solutions properly no or seser; accidents PREVIOUS AND a baEerialst gloves storing you have been vorking ava te IS should - reueDber: A fev Dg Dight your hands frequently vhen using r'ash outside Since air, liquids the vith reaction - - USE than occurs - THEIR la.boratory! safety of thoroughly described used incfude: contact case vash the heavy disposable in be SEPARATION IABORATORY ! ) I heavier nith These vear Dight none ventilation! norking prolonged avoid are a bottoD (i.e. in (Na- solutions and Clerici-solutioir), liquids hood acetone liquids Every - heavy NEW I{INERA]. of aequous Rohrbachrs- firbe TIIE affects hon-volatile daDage to EXPERIENCE, ACCIDEIflI RUIJS or RATE, AND/OR TIIE AI{Y ACTING equipDent inEediately. POTENTIAI. DANGER PERSON WITH NOT COI,IPLYING GROSS NEGLIGENCE SUSPENDED fROIi{ TIIE USE OF THESE FACILITIES! OF TIIESE WITA THE SHOI'LD BE geologist Re[ove foolhardy to fresh air (broDoforn), at once! If breathing has stopped use arti.ficial respiration! caII aDbulance iulediately and Dake Eure that label infomation. of soLution used is provided for further In case of Itinerals vith intoxication: having anorqanic rather high decolposed heavy liquids, aDounts by of reacti.on (zeolith, sDectite) reaet change their heavy density and incorporate are SoDe sulfide uirerals Detals. rith sol.utions containing heavy Detals. (acetonel ) can be incorporated into clay sone organic solvents [inerals alrd cau6e decrease 4. properbies ion-exchange in densitv. SEPAR-ATIONAPPARATUSFOR USE WITH HEAVY LIQUIDS: The sinplest nethod for separation is the use of funnel,s for nineraL separation. The setup consists of: a. the separatory funnel; b. a disDounta.bte filter c. Delbrane i a filter uhich can be evacuated flask, puDp. vater-otrrerated filter funnel vith a built-in separatory ceranic by connestion fiLter to a Both lhe heavy li.quid used and the sahple are introduced into the separatory funnel and agitated with a glass stirring rod. Dependent upon your grain size, density and viscosity of your you should not introduce rnore than a rlaxiDu.u of about heavy liquid o.sct! of sahplo materlal; as a rule you ghould start lrith barely covering the surface of the heavy liquid with grains - wait and to observe if the grains stj.ll or start clotting settle freely, each other preventing separation. You nay lhan (stepwise) add nore A11ol, than the uaterial, stirring the mixture after each addition. rnixture to conpleCely are and heavy fraction5 quite sorne tine, depending is It of the heavy tiquid. the stand until light separated. This Dight take upon volune, density and viscosity 2A advisable to trapped heavies a fairly bu t #4 ) ; the and passing papers nake rapid strength filter is laboratory filters) cerahic stopcock The the heavies using the vacuum system. process all liquid heavy bottle, the is use solvent or liquid in the heavy chenistry solution always use destilled unless filter After filter each apparatus: the liquids sieve Even both, be better or so of acetone. sanples had fumes the are (no - one uust use for drying! with !,/ater fune only or for containing cleaning heavy tiquid the to stock the are washed do positively vith of If other air and acetone had (lov and fastest (or hood do not any other the After lrashed ) I the solvent tapped have oven) contaDinate organic of the liquid. saDples been and speeds fractions Furthermore, acetone this staining!) the forget heavy explosive! safest (do not essential, (nixtures water funnel. grains returned the the the from as both To dry fil.ter not the and turning introduced is vacuun containing when flasks it volune the is <36,pn sizes funnel net!) under destilled liquid fron to by filter recovered funnels lab off to EIFE is - which is point) inethod tapped trough a greater used boili-ng Whatrnan s in c e grain by pass done acetone/methanol/ethanol been the sieve-net (e.g.: appears Than a new filter IR-lamps, ttten all PIFE e s p e c ia lly paper clogged to tapped. water the n ic e L y , than tapped, best filter destilled not is and recovers the vith are paper process fi.l.ter allow paper filter filter are them the renaining do get heavies filter to as fast to and allowing insert grade coffee tirice After to ti)nes (preferably a fil.ter will nenbrane (<400nesh). several than the laboratory grade filter 1/ao are about only the cost as e.g. Whatnan #4 is inserCed into the filter funnel to prevent and they - sure laboratory of tine Lights sink. a coffee wet the to the proceeding, Before or agitate been sanples renoved funnels ! separation Use destilled one water llust first, thoroughLy than clean acetone ttle (fune - vttole hood!), 29 process! Never leave used separation of Narrill result in precipitation uncleaned as this in the fj.Lter ueDbrane, polytungstate on the rtalls and especially ! ntrthenore, insoluble Ca-polytungstates turn into uhich night allov to glassrrare turn the fLasks, . 5. dry filter before next punp off, nake sure IR-bulbs aLlolt air are snitched systeD fill off (tiDerl). to and filter REIARKS: for Producing pure The above-degcri.bed netbod is not satisfactory particutarly and is tine-consuldng. nith fine naterial separates. are needed ttith a resultant large voLuues of llquid Furthernore, ttle Hosever. witb each separation. of Dore heavy liquid loss Na-polytqngstate, non-toxic of coDparably cheap, avail.ability has qreatly toxic heavy liquids, of the connon, highly instead overco[es both of Centrifuqling i.Dcreased the use of this [ethod. is nat in but the ttide use of the centrifuge these difficulties. rotor tubes and reinforced because the special evidence nainly expensive. and are therefore axeg needed have to be custoE-built