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The Structure of Bayldonite: Chemical Analysis, Differential Thermal

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The Structure of Bayldonite: Chemical Analysis, Differential Thermal American Mineralogist, Volume 66, pages 148-153, IggI The structure of bayldonite:chemical analysis, differential thermal analysis,and IR spectroscopy VerBNrrNn SuuiN DE PoRTTLLA Instituto de Geofnica, UNAM Mbxico 20. D.F. MeNuer PoRTTLLA Quevnoo Institut o P o lit i cnic o N acional Mdxico. D.F. AND VICToR I. STEPANoV I MGRE, Moscow, U. S.S.R. Abstract Chemical analysis,differential thermal analysis,and IR spectroscopyshow that the struc- ture of bayldonite lacks water molecules and contains OH groups coordinated with Cu atoms,as well as acid arsenateanions (HoAsor)'z-. The H bondsformed by the hydroxyls of the (HOAsOr)2- groups are very short and strong,with the possibleappearance of a tunnel effect for the hydrogen atom. The formula CurpbO(HOAsOr)r(OH), is proposed. Introduction 77o!l; a:b:c: 0.843:l:l.16l.The crystalwas opti- cally positive with la;ge 2V. The refractive indices Bayldonite is a Pb-Cu arsenatewhose structur€ were:y : 1.99-10.01,B : 1.98,a: 1.94(Guillemin, has not been established.Most samplescome from 1956).The calculatedvalue (-) 2V: 52oshows that Tsumebin SW Africa, whereit is found in the oxida- at least the value of B must be wrong. The resultsof tion zone of this deposit (Guillemin, 1956;Frondel Larsen:y : 1.99,B : 1.97,a: 1.95give -2V : 89", and Ito, 1957).Bayldonite has also been found in which could be a tolerable error. France: Verriere, Ardillats, R6he, Rebasse,Ceilhes, Bayldonite can be synthesizedat l80oC and a pH Herault (Guillemin, 1956);England: uranium mine, between5 and 8. At this temperatureand at a pH of Grampound Road, Cornwall (Guillemin, 1956);and 7, bayldonite is formed from schultenite(HPbAsOn) the USSR,Dzeskazghan (Satpaeva, 196l). This min- in the presenceof Cu(NO.)r, or from a solution of eral was describedby Church (1856)from St. Day, HrAsOo, malachite, and cerussite.When the pH is Cornwall. lowered to 34, duftite [CuPb(AsO,XOH)]is formed Guillemin (1956)compared the chemical analysis (Guillemin, 1956). of synthetic and natural bayldonite, and gave a Cu:Pb relation of 3:l as reported previously by Mineralogical studies Church (Table l). However, the agreementbetween Bayldonite used in this study occursin the oxida- the proposedformula and the analysisis unsatisfac- tion zone of a metasomatic Pb-Zn deposit in Kay- tory, especiallythe excessof water moleculesfrom rakty in central Kazakhztan It was found in the up- the analysis. The optical properties of bayldonite per layers of barite lenses of considerable size (Larsen, 1921,p.45) showedthat this mineral has embedded in sandstone.Bayldonite is formed by monoclinic symmetry.This wasconfirmed by Guille- pseudomorphicsubstitution of cerussite,resulting in min (1956),using X-ray methodson a samplefrom irregular accumulations in fine-grained malachite Cap Garonne. The parametersof the unit cell are:a and azurite. Concentric accumuliationsof pure bayl- : 5.03+0.02,b : 5.97+-0.05,c : 6.93+0.02A,B : donite reacha diameterof -7 cm. Occasionallybayl- 0003-oo4x / 8| / 0I 02-0I 48$02.00 SUM|N DE PORTILLA ET AL: STRUCTURE OF BAYLDONITE 149 donite is found on thick spherolite-likecrusts formed choidal fractures.The separationof Pb and Cu was in fractures in the barite. Concretions of bayl- problematic due to the sensitivity to pH. The results donite (up to 3 cm in diameter) in clay layers inter- of chemical analysisare given in Table l. bedded with sandstonewere also observed.In these concretionsconcentric color patternsoccur due to al- IR spectroscopy teration in the compactnessof the material. Bayl- The IR spectrawere recorded on a UR-20 Zeiss donite has a characteristicapple-green color with a infrared spectrophotometer(DDR). The samples yellowish hue. Dense aggregationshave an intense were prepared as emulsionsin nujol on NaCl win- oily luster and show conchoidal fracture. The less dows. Deuteration of the sampleswas carried out in dcnse type is dull with an irregular fracture. The an autoclave at pressure -15 atm and at temper- dense bayldonite often shows cavities with small atures from 200o up to 500"C for a minimum of 48 crystals of anglesite and azurite. Both types of bayl- hours. Two sampleswere used, one from Tsumeb donite usually intergrow with beudantite, PbFe3- and another from Kayrakty. (SO)(AsO.)(OH).. Microscopicexamination of grain immersion mounts and thin sectionsof bayldonite D iffer ent ia I thermal analys is showsa microspheroliticstructure of bayldonite ag- gregates.The densetype is homogeneousand some- DTA was carried out in a Paulik Erdel rneo-58 times small inclusions of anglesitegrowing on DR analyzer.The samplesweighed 0.4 g and the rate spherolitesof bayldonite may be observed,while the of heatingwas 5oClmin. lessdense is more heterggenous. Results Chemicalanalysis The data of the chemical analysis reported in The microchemical analyseswere carried out in Table I were used to calculate two empirical for- the Institute of Geology of Mineral Deposits,Miner- mulas for bayldonite. alogy, Petrography,and Geochemistryof the Acad- (l) Bayldonite from KayraktY: emy of Sciencesof the USSR. Samples used for chemicalanalysis were apple-greenand showedcon- Cu. -Pb, *(AsOo),nr(POo)o or(OH), or'0.74Hro Table l. Chemical analysis of bayldonite I 2 2 3 3 4 4 Relation Relation Relation of atomic of atomic of atomic Oxides nrr-hfi+i6c weight % Weight Quantities Weight % Quantities weight ? CUO 31.61 31.70 2.996 30.88 2.968 32.5 2.98 Pbo 30.30 32.60 1.004 30.13 1.032 32. L 1.049 As^O- 3L.20 30.09 1.968 37.76 2.LI3 JI. f, 2 z) DO 0.20 o.02L z1 tt^o+ 4.89 4.20 3.504 4.58 3.887 3.00 3 so- 1.00 J CaO 2.65 z5 100,00 99.79 100.00 99.8 q, 5.24 Lt 1.- Cu- Pbo (HASO,)^ (Calculated) 2.- Kafrakty, cenLr1I Kazakhstan, USSR 3.- St. Dayf Corni^/all (Church, 1865) Cit, after Dana's Svstem of Min., 7th ed. 4.- Synthetic Bayldonite (cuillemin, 1955), 150 SUMIN DE PORTILLA ET AL: STRT]CTURE OF BAYLDONITE 600 700 1100 1300 1500 1700 1900 2100 2300 2500 2700 2900 3100 3300 3500 o o z. 9 F o- E o !n @ Fig. I IR spectra of bayldonite (in nujol): (a) Tsumeb; (b, c) Kayrakty. * : bands of nujol (2) Bayldonite from Cornwall: (Fig. I, Table 2) in the zr(Tr) region of the arsenate anion. This band is split into four components: 780 Cur rrPb,o.(AsOo), ,,(OH), ur.l.l lHrO cm-', 815 cm-', 840 cm-, and 870 cm-'. In the defor- For the synthetic compound we obtained the for- mation vibrations region zo(Tr), the same kind of mula: splitting appears with three maxima: 400 cm-', 440 cm-', and 475 cm-t. The z,(Ar) band is very sharp Cu, nrPb,or(AsOo), oo(OH)2 *.0.4j HrO and intense. The 1060 cm-', 1090 cm-', and ll20 From these results we conclude that the formula cm-' do not shift after deuteration (Fig. 2) and are Cu.Pb(AsOo)r.(OH), cannot be correct. The two em- probably due to zr(Tr) vibration of the phosphate an- piric formulas suggest that bayldonite contains a wa- ion which is present in bayldonite. The z,(A,) band ter molecule: Cu.Pb(AsO"),(OH),.HrO. of the phosphate anion also appears at970 cm-'as a The IR spectra of the samples of bayldonite from weakly defined shoulder. In the Me-O (Me : metal) Tsumeb and Kayrakty both show an intense band stretching vibration region only Cu-O vibrations are Table 2. Frequencies of absorption bands in the IR spectra of bayldonite and tentative explanation of the absorption bands ?- -3 tr t- Aso4 \ or.f I -tI Cu-OH ,lOH...O 2v 5:' L ["", oo ] OE cu-o 6oH Byaldonite from Tsumeb J. ta, I )3(r2) )4 (r2) ) /m \ \ r- r and Kayrakty ' t \r(ar) V?\rrl V/\ftl ABCD I )U 780 400 970 1060 562 700- NNFP s OOtsO6 815 440 1090 18s 8oo 3 Freguencies, 840 475 -1 r720 cm 870 (s40) u O ( ) Numbers in parentheses represent frequencies of absorption bands of deuterated samples. SUMIN DE PORTILLA ET AL: STRI]CTURE OF BAYLDONITE l5l r000 12C0 1,100 1600 )800 240A 2600 2800 3000 1200 3400 I600 o o z t- a- E. o a CD * Fig. 2. IR spectra of deuterated sample of bayldonite from Kayrakty (a, b different concentration of bayldonite in nujol) : bands of nujol. expected, due to the covalent nature of this bond. Discussion The vibrations of the Pb-O bond do not appear in The structure of bayldonite is unknown. From the predominantly the IR spectra because of its ionic chemical analysis of bayldonite from Kayrakty we character. Two sharp bands at 562 cm-' and 585 conclude that the empirical formula Cu.Pb cm-' occur in the IR spectra of bayldonite. Analo- (AsO.),(OH), given by Guillemin (1956) lacks two gous bands are present in the spectra ofolivenite and hydrogen atoms and an oxygen atom. The search for conichalcite (Sumin de Portilla, 1974), and, euchroite a possible water molecule in the structure of bayl- and liroconite (Sumin de Portilla, unpublished re- donite is important in order to establish the correct sults). These bands are related to vibrations of the chemical formula. The IR data were mainly used to Cu-O bonds. The zo(Tr) band for the phosphate an- answer this question. The splitting of the z.(T') and ion does not appear in the spectrum. A band with zo(Tr) bands in three components and the appearance very low intensity occurs at 1650 cm-' in the defor- of a z,(A,) band in the spectra of bayldonite clearly mation vibration region of water.
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