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TINTINAITE,I THE ANTIMONY ANALOGUE OF KOBELIITE
D. C. HARRIS,2 J. L. JAMBOR,S c. R. LACHANCE,8 R. I. THORPE4
AssrRAcrRe-examination of kobellite, a Pb-Bi-Sb sulphosalt, from the type rocality, Hvena,
Sweden, and from three new North American localities has led to a redeiniiion of themineral ?19 t!" discovery of its new antimony analogue. Electron probe analyses showthat a solid solution series is present and extends from the high bismuth member to thepure allimony end-member. The ideal formula for the kobel-lite series is 5pbs.4(X)2s,where X is Bi andlor Sb.
The structural cell is orthorhombic with space group pnnm, The unit-cell dimensions,as determined by Nuffield (1948) forkobellitewith approximatelyTo/68i, areo :22.62,D : 34.08, c : 4.02 A, while tiose of the pure antimony membir from Tintina, yukonjare a:22.30, b : 34.00, c : 4.04 A. Densities of the minerals in the series increasefrom 5.47 for tle antimony end-member to 6.gg for the bismuth end-member.-.It-is proposed that the name kobellite be retained for minerals in the series havingBi:Sb : )1:1, and that antimony-rich members (Bi:Sb : (1:1) be assigned the neiname tintinaite.
INrnonucrrolr
Kobellite was first identified and named by setterberg in L88g from thecobalt mine of Hvena, Sweden. In his description, Setterberg proposed aformula of Pbr(Bi,Sb)gSo with Bi:Sb : -2:L. However, Rammelsberg(1875) rejected Setterberg's analysis and, on the basis of analyses byhimself and Genth, he deduced the formula Pba(Bi,Sb)rSo. Keller (1Sgg)Iater reported a new occurrence of kobellite at the silver Bell mine,ouray, colorado, and from the analysis of this material he confirmed theoriginal formula proposed by setterberg. on the basis of this early work,the mineral is given in Dana's System of Mineralog'y as a doubtfulspecies of unknown crystallography and composition, possibly pbr(Bi,Sb)2S6. The proposed formula for kobellite is thus equivalent to anantimonian cosalite (PbrBirst to which it is very similar in physicalproperties.
Beyond this original work, very little had been added to the descriptionof kobellite until Nuffield (1948) showed by single-crystal and r-raypowder methods that the Hvena kobellite was not merely an antimoniancosalite but was an independent species. on the basis of the two earlierunsatisfactory analyses by setterberg and Keller, and with a new specificgravity measurement, Nuffield suggested 6PbS.FeS.2Bi2SB.Sb2Sg &s. ?
rrhe name has been approved by the commission on New Minerals and MineralNames, I.M.A.
zMines Branch, Ottawa, Ontario.sGeological Survey of Canada, Ottawa, Ontario.aGeological Survey of Canada, Yellowknile, N.W.T.
372 THE CANADIAN MINERALOGIST
tentative formula until the question of cell contents could be settled by a
new and reliable analysis.
Marnnrar,s Srunrpo
In addition to the Hvena (Sweden) and Ouray (Colorado) occurrences,kobellite has been reported from five other localities (Table 1), but in noneof these has an attempt been made to settle the question of cell contents.
The r-ray identification of kobellite from the dump of the Deer Parkmine in the Rossland area of British Columbia (R.I.T.) and from theTintina Silver Mines, Tintina' Yukon (Hunt, 1964) provided an oppor-tunity to make new observations on this mineral. The following additionalspecimens labelled as kobellite were also examined: U.S.N.M. C'754,Leadville, Colorado; U.S.N.M. R-1025, Old Lout mine, Ouray, Colorado;H.M.M. 82436, Red Mountain, Colorado; National Mineral Collection(Ottawa) specimen 7101, Ibex mine, Leadville, Colorado;U.B.C. speci-men from Dodger Tungsten mine, Salmo, British Columbia. X'raypowder difiraction and polished section studies of these specimens showedkobellite to be present only in the Salmo material. In addition, however,Paul Desautels of the U.S. National Museum kindly provided us withkobellite from another new locality, Raleigh, North Carolina.
Dnscnrprrort or NPw OccunnoNcpsRosslnnd,, B.C.
Kobellite was identified in a specimen collected from the dump of theDeer Park mine by one of us (R. I. T.) during the course of a minera-logical investigation of the ores from the district. Identification was made
by its r-ray powder pattern and was confirmed by determination of itsoptical rotation properties. At this locality kobellite occurs as bladesenclosed in granular qlJartz. The blades in some cases form parallelaggregates which are up to 2 mm long by approximately 0.5 mm across.Less commonly, fine blades form somewhat radiating fibrous clusters.Subhedral to euhedral crystals of pyrite and arsenopyrite are associatedwitJr the kobellite. In some specimens the mineral is also closely associatedwith small amounts of pyrrhotite, chalcopyrite and magnetite.
Native bismuth, intergrown with galena, has been identified from alocality only a short distance northeast of the Deer Park deposit. Otherbismuth and antimony-bearing minerals-bismuthinite, galenobismutite,and boulangerite, are found elsewhere in the Rossland camp.
Specimens of the Rossland material are catalogued in the RoyalOntario Museum Collection, Toronto, Ontario x M27L73, M27L74,M27L75,M27L76.
TINTINAITE FROM TINTINA, YUKON
Tasr,B 1. Locar-rtrps ron Kospr-r.nr
Occurrence Reference Commmts
373
Hvena, Sweden
Ouray, Colorado
Boliden deposit,Sweden
Dodger TungstenMine, Salmo. B.C.
Ustarasaisk deposit.Russia
Jilovd area,Botremia
Central SoanishPyreneis
Keller 1889
Odman 1941
Thompson 1954
Sakharova 1955
Mor6vek 1956
van der Lingen J.960
Associated witltpyrrhotite, chal-copyrite
All analysesaverageT-8/sA g f C u * F e * Z n
Both Bi and Sbsulphosalts present.
Analysis showsSToFe
Associated withbismutlian robinsonite
X-raypowderdatalisted; Bi andSb indicated byspectroscopy
With arsenic-bearineminerals and native Bi.Identificationtentative
Setterberg 1841;Nuffield 1948
T,i,nt'i,na S'i,hter M,i,nes, VukonDuring the course of a mineralogical investigation of ore specimens
from Tintina silver Mines by Hunt (1964), a mineral identified by r.raypowder photographs as kobellite was reported. The mineral occurs assmall masses measuring up to 2 mm in diameter and as veinlets fillinginterstices and fractures in malachite-stained weathered quartz. Likekobellite from sweden, its colour is lead-grey, it has a black streak and ametallic lustre. The (010) cleavage is well developed. Micro-hardness.wasdetermined to be C- (Talmage).
The principal associated mineral is jamesonite. Additional mineralsidentified in the area were argentian tetrahedrite, galena, sphalerite,pyrite, arsenopyrite, marcasite, bournonite, owyheeite, pyrrhotite andchalcopyrite, with the first three being the most abundant. It is interestingto note that none of the sulphosalts are bismuth-bearing.
The specimen of the Tintina "kobellite" kindly donated to the writersfor this study by Miss Hunt is catalogued in the systematic collections ofthe Geological survey of canada while other specimens are catalogued inthe research collections of the Department of Geology, university ofToronto.
Swperior Stone Quarry, Ral,e'i,gh, Nmth Carol,inaThe specimen of kobellite (u.s.N.M. 11gzg6) from this locality was
374 TEE CANADIAN MINERALOGIST
identified originally by John S. White Jr., Division of Mineralogy,
Smithsonian Institution.The quarry is located in wake counry and is also known as the
Crabtree or Nello Teer Quarry. Although Mr. White has not visited the
locality (priv. comm.), he reports that the "kobellite" appears to occur in
richly mineralized granite pegmatite veins associated with bismuthinite,jamesonite, and tetrahedrite. Other common minerals in the seams are
chalcopyrite, pyrite, siderite, tourmaline, garnet and rutile. Small vuggy
areas contain- well-formed crystals of monazite, muscovite, rutile and
barite.The small unattached grains provided for this study contained only
bismuthinite, tetrahedrite and kobellite. Partial electron probe analysis of
the bismuthinite gave approximately L5/p antimony. weissenberg single-
crystal photographs of this material gave cell dimensions a : tl.lz,,
b : 11 .30 , c : 3 .96A*co-p t ed toa : 11 .15 , b : LL '29 ,c : 3 '984
for pure bismuthinite.
Er.pctnox Pnoss ANer-Ysrs
Kobellite occurs in such small quantities and intermixed with other
physically similar minerals so that the only reliable method of determin-
ing its composition is with the electron probe. In this study, four speci-
-"nr pron"d suitable for analysis, the results of which are given in
Table 2.The only specimen not a1.alyzed at the Geological Survey of Canada
was the one from Hvena, Sweden, which was analyzed by J. C. Rucklidge,
Department of Geology, University of Toronto.ihe results of the analyses show that a solid-solution series is present,
extending from the high bismuth content of the Swedish material to the
pure antimony end-member from Tintina. The Rossland and the North-Carolina
specimens occur in the middle of the series with the former being
closer to the antimony member. The compositions of these four minerals
clearly show that a continuous series is probably present'
The atomic proportions derived from the analyses (Table 2) show a
variation in the Pb:(Bi,sb) ratio o<tending from L:L.24 to a high of
1:1.61. For this range of values, it is possible to deduce only two cell
contents which approximately correspond with the unit-cell and specific-
gravity mez6urements, namely 10Pbs.7(x)2s3 and sPbs.4(x)rSa where
? ir gi and/or Sb. For the pure antimony (Tintina) member, the calcu-
lated densities for 10PbS.7sbrSa and 5PbS.4SbrS3 ?rel r€sp€ctively, 5'111
with Z : 2, and5.475 with Z : A.The predicted density (Jambor, 1967)
of l0PbS.7SbrSg is about 5.60, whereas the predicted value for
TINTINAITE FROM TINTINA, YUKON
Tanr,B 2. MrcnornosB ANer.vsps aNo DsNsrrrss on MursRALs
375
rN tge Kossr,r.trB SBntss
Weight%
Raleigh,N.C.
Hvena,Sweden
Rossland,B.C.
Tintina,Yukon
PbBisbCuAgFes
33.237.69 . 61 . 00 . 50 . 6
18.6
38 .028.5':'
L8 .0
42.323 .0L7 .6n.d.*n.d.n.d.20.0
42.3n.d.34 .5n.d.n.d.n.d.2 L . 3
Atomic Proportions:PbBisbs
Atomic /o Bismuth intlre.(Bi, Sb)posruon
Calculated DensitvfMeasured Density
'
102.9
5 .002 .70 \ 6 .203 .50 r
15.30 '
43.56 . 16
98 .1
5 .000 .00 \ 6 .906 .90 J
16.30
0 .005.48D . D I(predicted)
5 .00 5 .005 .601 8 .05 3 .70 . I 7 .052 . 4 5 1 3 . 3 5 1
18.10 L5.25 '
10t .1
6 9 . 66 . 5 16.48
99 .5
52.46.276 .31
*Not detected.-JQ"qsltisl calculated from the analytical Bi:sb ratios substituted in t-he formula5PbS.4(X)rS8.
SPbS.4SbrSa is about 5.51. The latter formula is therefore the obviousselection.
X-nav Cnystar,r.ocRApuy
Rotation and weissenberg *-ray difiraction studies by Nuffield (1g4s)showed that the Hvena, sweden, kobellite was a distinct species havingorthorhombic symmetry with cell dimensions of a : 22.62, b : 84.0g,g : 4ao2 A, space group Pnrnm.The results obtained in the present studyfrom weissenberg and precession examination of kobelliies from fouradditional localities are listed in Table B.
The films confirm the orthorhombic symmetry, but only the salmomaterial gave the space group Pnmm. Photographs of material from theother three localities showed that the conditions for non-extinction were0klwithb + I : 2n,h\l,withk * I : 2n,givingaspacegroup of. pnnmor Pnn2. This difference in space group is due only to the systematicextinction of the h\I reflections which, in the weissenberg films, are verypoor. Since the space group Pnnrn is the most common in this series, the6lms obtained by Nuffield of the sweden material kindly were lent to usfor a closerstudy. comparing these films with those obtained in this studyindicated that Pnnm is more likely the space group for the mineral fromthis locality.
376 TEE CANADTAN MlNERALoGrsr
Test-e 3. Ur.in-cBr,r- Dere non lus KossLLtrB SBmBs
Salmo,Hvena, B.C.Sweden (This
(Nufreld) study)
Raleish. Rossland, Tintina,N.C-. B.C. Yukon(This (This (This
siudy) study) studY)
abc
Volume
SpaceGroup
zCleavage
22.62 L34.084 .02
3099 .0 A8Pnnm
orPnmm
22.56 A34.004.04
3098.8 As
22 .$ A3&.974 . M ^
3092 .0 A8
22.50 A 2230 A34.00 34.004 .03 4 .M-
3082.9 fu 30ffi.1 A8
Pnmrn Pnnm Pnnm Pnntn
4 4 4 4010 010 010 010
4010
The other important feature of the single-crystal study is the variationin unit-cell dimension a from the pure antimony end-member to the high
bismuth member. This relationship is illustrated in Figure 1 which shows
o versus the atomic percent bismuth in the (Bi'Sb) position.As can be seen, the graph shows a linear relationship up to 75/s Bi
which could probably be extended to the pure end-member. The variation
in the a cell dimension with change in composition may be distinct enough
so that the o value can be used as a measure of the amount of Bi in the
t o 2 0 3 0 4 0 5 0 6 0 ( s 5 u w
ATOMIC PER CENT Bi
Frc. 1. Shows the variation in unit-cell dimensions @ versus atomic percent bismuth in
the (Bi,Sb) position.
. <
zIu,zlrlt6g
TINTINAITE FROM TINTINA, YUKON 377
(Bi'sb) position. This correlation with the single crystal data may befortuitous, but is amazingly good considering that ihe unit-cell valueswere not all determined in one laboratory. In an attempt to obtain moreprecise unit-cell dimensions, the powder data were run through a refine-ment programme givjng values for the Tintina material of. a : 22.89,b :34.OZt c:4.04A and the Hvena mater ial , a:22.56, b : BB.g4,c : 4.02 A. In the refinement programme, it is possible to derive quitedifferent unit-cell dimensions depending on which indices are included.For this reason, the r-ray powder data are not considered to be sufficientlyprecise to warrant further refinement. The refined unit-cell values weretherefore only used for indexing the Tintina and Hvena powder patterns.
Although microprobe analyses of the salmo mineral could not beobtained, the above graphical relationship indicates that its Bi contentwould be about 55-60 atomic percent, close enough to suspect thepossible presence of an ordered compound with Bi:Sb: L:1. This,however, is at variance with the reduction in space-group symmetry fromPnnrn to Pnmm. As only one single-crystal fragment of poor quality wasexamined, further study is clearly needed before any meaningful con-clusion can be reached.
X-nay Powpsn Drmru.crroN Dara
x'ray powder data for the minerals examined in this study are given inTable 4. All measurements were made on films obtained with 1r.4.6 mmdiameter cameras and nickel-filtered copper radiation. The only reason-ably distinctive pattern in the series is that of the pure antimony end-member from Tintina. A characteristic feature is the appearance of amedium strong reflection at 2.022(6) which appears as a doublet (2.089and 2.019) on the other patterns.
Dnnsnv
In the original description of kobellite from sweden, setterberg (lgal)determined the density to be 6.2g-6.88. Nuffield (194g) was able tomeasure with a Berman balance several clean fragments from this localityand obtained a value of 6.48 + 0.05. In the present study, only the Northcarolina specimen proved suitable for density measurements. Two frag-ments (total weight 5.5 mg) taken from a polished section were measuredon a Berman balance by H. R. Steacy, of the Geological Survey ofCanada, and a value of 6.BL was obtained.
As the microprobe analyses of each element (Table z) are subject toerror, only the analytical Bi:sb ratios have been substituted in the
THE CANADIAN MINERAI,OGIST
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TINTINAITE FROM TINTINA. YUKON
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380 THE cANADIAN MINERALocIST
formula 5PbS.4(X)rSg for the purpose of calculating the densities of the
minerals. For kobellite from Hvena, Sweden, the calculated density is
6.5L, in excellent agreement with the measured value of 6.48. Likewise'
the measured and calculated densities of the North Carolina kobellite
(6.31 and 6.27 respectively) agree well.The effect of bismuth content on density throughout the Bi-Sb series is
graphically shown in Fig. 2. The predicted density of the end-member
compound 5PbS.4Birsg is 6.99.
to 20 30 40 50 60 tO uQ
ATOMIC PER CENT Bi
Frc. 2. Shows the relationship between calculated density and atomic percent bismuthin the (Bi,Sb) position.
Rorerrou PnopsnrrBs AND REFLECTTvTTIES
The only specimen on which rotation and reflectivity measurements
were made was the Rossland material. The rotation angles and phase
differences were measured at a series of wave-lengths using established
techniques (Cameron, 1961), and the results were in essential agreement
with the recorded values for selenium-bearing kobellite from Sweden (van
Rensburg & Cameron 1965). At a wave-length of 546 mp the rotation
angle, Ar, and phase difference, 20, were determined to be 1.84o and
0.8ot, respectively.
TINTINAITE FROM TINTINA. YUKON 381The approximate uniradial reflectivities at a waveJength of 546 mp are
as follows:Rp 36 .6Rrn 39.0 to 41.1Rg 45.4
They were measured using silicon and tungsten as standards, withreflectivities at this wave-length ol 87.0/s (NpL Report, ReferenceN2538, August 22, 1966) and 53.3/s, respectively. Only seven grainssuitable for measurements were present in the polished section preparedand the value of Rrn could only be determined to lie between}g.O/s and4L.LT,. However, the mineral is almost certainly optically positive(Cameron,1963).
calculation of the reflectivity ratio R2/Ry from the measured rotationproperties (Berek L953) gives a value of 0.87g. This gives a calculatedvalue of 39.9% f.or Rp, which is much too great. There is thus a conflictbetween the measured uniradial reflectivities and rotation properties.some errors in reflectivity are to be anticipated due to the great numberof factors which influence the measurements. However, even if maximumand minimum values are rejected as erroneous (giving values of. BZ.5/sand 44.4/s f.or Rp and Rg, respectively) the ratio of Rp and, Rg is onlyincreased to 0.845, which indicates that the measured rotation angleshould be as great as 2.42".It seems probable that the rotation propertieshave not as yet been determined on a grain with the proper orientation togive maximum values.
Nounuclarunu
The minerals described here are apparently members of a continuoussolid-solution series with the general formula 5Pbs. 4(x)rss where x is Biand/or Sb. The series may be arbitrarily divided at the Bi:Sb : L: L, withminerals in the bismuth-rich portion being assigned the name kobellite.N{inerals in the antimony-rich portion are assigned the new nametintinaite, the name being derived from the locality for the antimony end-member. It is also suggested that the solid-solution series be referred to asthe kobellite series.
The formula proposed in this study for tintinaite, namely bpbs.4Sb2Ss,is identical to another rare sulphosalt mineral, plagionite. However, thetwo minerals are structurally different. Plagionite has cell dimensionsa : L 3 . 4 5 , D : 1 1 . 8 1 , c : L g . g A , B : L 0 7 o l L , s p a c e g r o u p C 2 / c a scompared to tintinaite of dimensions o : 22,30, b : 34.00, c : 4.04 A,space group Pnnm. In this respect, the minerals are to be considered asdistinct species.
382 TEE CANADIAN MINERALOGIST
Acrnowr-nocMENTs
The writers are indebted to P. Desautels, C. M. Hunt, R. M. Thomp-son, and H. R. Steacy for kindly providing kobellite specimens for thisstudy. The assistance of R. N. Delabio in the preparation of. x-tay powderpatterns, J. C. Rucklidge for the electron probe analysis of the Swedishkobellite, and H. R. Steacy for its density measurement is gratefullyacknowledged.
Rnrpnpxces
Brnnr, M. (1953): Nnne-Berek Anl,eitung zu opt'i'schm Untersuckungan m'il d.em Pol'ar',isat iansmihros&op : E. Schweitzerbart'sche Verlagsbuchhandlung, Stuttgart.
CeuenoN, E. N. (1961): Ore M'i,croscopy: John Wiley and Sons Inc., New York' 293 p.(1963): Optical symmetry from reflectivity measurements: Am. M'ineral, 48,
1070-1079.Huut, C. M. (L964): A study of lead-zinc silver mineralization at Tintina Silver Mines,
Yukon, M.A, Thesis, Unin. Toronto.Jeunon, J. L. (1967): New lead sulfantimonides from Madoc, Ontario-Part I, Can.
M'i,neral',9,7-24.KBr-r-en, H. F. (1SS9): Ueber Kobellit von Ouray, Colorado, und Uber die chemische
Zusammensetzung dieser Species, Z ei'ls. Krist., 17,.67-72.MonAl,rr, P. (1956); Vizrnutovd miner6ly ,e Slojiiskd Zily v oblasti dolu Pe[r u
jiloveho (Bismuth minerals from the slojii vein in the area of the Pepi mine near
Jilove), Casopi,s pro min. geol,,,1,223-232.Nwrrslo, E. W. (L948): Observations onkobellite, Un'iv' Toronto StuiL'ies' Geol'. Ser.,
52, 86-89.oouaN, O. (1941): Geology and ores of the Boliden deposit, Sver. Geol'. Unders., Arsboh,
35, 1-190.ReMMpr.sspnc, C. F. (1875) : Hanilbuch d'er M'i'neralchem'i*, 2nd edition.Sexsenove, M. S. (1955): On bismuth sulphosalts of Ustarasaisk deposit, Trans. Miner.
Mus., Acol'. Sc'i'. U.S.S.R., 7, tL2-126.Srttennonc, (L8/1)z (Ak. Stochkol,m, Hand,l.,27, p, !88, 1841 for 1"839) See Nuffield,
1948.TuoupsoN, R. M. (1954): Mineral occulrences in western Canada, Am, M'i'n., 39,
525-528.vAN DER LrNGeN, G. J. (1960): The arsene-bearing copper ores of Canfranc Estacion
(central Spanish Pyrenees), Geol'. en Mijnbouw, 22, 72V736.veN RBNssuRo, W. C. J., & CauBnoN, E. N. (1965): Additional data on rotation
properties of ore minerals II: Ec'Ge01,.,60,L718-1720.
Manuscr,ipt recehted, September 21 , 1967, ernended December 1, 1967