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Profesionăˇlnă Referăˇt Journal of the Czech Geological Society, 42/4 (1997) 77 New naturally occurring phases of secondary origin from Jáchymov (Joachimsthal) Nové sekundární minerální fáze z Jáchymova (Czech summary) PETR ONDRUŠ1 - FRANTIŠEK VESELOVSKÝ1 - ROMAN SKÁLA1 - IVANA CÍSAěOVÁ2 - - JAN HLOUŠEK3 - JIěÍ FRÝDA1 - IVAN VAVěÍN1 - JIěÍ ýEJKA4 - ANANDA GABAŠOVÁ1 1 Czech Geological Survey, Klárov 3, 118 21 Prague 1 3 The Faculty of Science, Charles University, Hlavova 2030, 128 43 Prague 2 2 U Roháþových kasáren 24, 100 00 Prague 10 4 National Museum, Václavské námČstí 68, 115 79 Prague 1 This paper describes thirty inorganic compound – secondary mineral phases- found in the nature for the first time. All compounds come from the Jáchymov ore district. All up-to-now available physical and chemical data and references to appropriate literature are given. Crystal structure of phase [ (MoO2)2As2O5(H2O)2] . H2O was solved and refined, crystal structures of Ca(H2AsO4)2 and Mg-villyaellenite were refined by the Rietveld method. Key words: new natural phases, new data, secondary minerals, Jáchymov Introduction Single peak profile fitting procedure using Pearson VII split asymmetric profile shape function implemented In the course of work on the project Study of secon- in the program ZDS ver. 6.01 [291] found angular posi- dary minerals in the Jáchymov ore district (1993 to tions and intensities of reflections in the powder pattern. 1997) [299] we have recognised and studied 30 inor- Diffraction indices were assigned to yielded reflection ganic phases, which were for the first time encountered positions based on theoretical powder pattern calculated as natural materials. This development prompted us to from the crystal structure data with program FullProf write this paper, dedicated exclusively to the new phases. (version 3.2 for PC-compatibles - [284]). Individual phases are characterised to variable degree, Lattice dimensions were refined from those data with depending mainly on the type and quantity of material program by Burnham [281] employing correction term available. (cosTcotT)/O2 for sample displacement. In the case of CAS and "Mg-villyallenite", program FullProf (version 3.2 for PC-compatibles - [284]) was Experimental methods used for the Rietveld refinement of crystal structure of this new mineral from experimentally measured powder The experimental methods used in study of the new X-ray diffraction data. Background was approximated phases are the same as characterised in the paper pre- via polynomial of the fifth order, corrections for sample senting encyclopaedical review of Jáchymov minerals: displacement (cosine term) and preferred orientation (in Secondary minerals of the Jáchymov ore district. Addi- March-Dollase form) were applied. Pseudo-Voigt profile tional methods used in study of the new phases include shape function was utilized. Peak base was set to 5.5 single crystal study and the Rietveld analysis of three FWHM. new phases: [(MoO2)2As2O5(H2O)2] . H2O (provisional For the single crystal X-ray measurement a needle- designation MOASO), Ca(H2AsO4)2 (provisional desig- like fragment of MOASO was mounted on a glass fibre nation CAS) and "Mg-villyallenite". and measured using the four-circle diffractometer Powder data (for Rietveld analysis) were collected CAD4-MACHIII with MoKD radiation. The crystallo- using Philips X'Pert diffractometer equipped with copper graphic data obtained are summarised in Tables. The sealed tube and graphite secondary monochromator. crystal structure was solved by direct methods High voltage was set to 40 kV and tube current to 40 (SHELXS86 [287]) and refined by a full-matrix least- mA. Powder pattern was collected in range from 3 to square procedure based on F2 (SHELXL93, [288]). Scat- 120 °2TCuKDand step 0.01 °2TCuKDwith exposition tering factors were those employed in the SHELX pro- of 10 sec. per step for CAS and in range from 3 to grams. 130.005 °2TCuKD with step 0.015 °2TCuKDand ex- The qualitative, and in some cases quantitative, position of 10 sec. per step in the case of MOASO. To chemical composition of minerals was measured with minimize complicated shape of background due to clas- the scanning electron microprobe CamScan 4 with an sic glass sample holders, the sample studied was placed energy-dispersive analyser EDX system LINK eXL and on the surface of flat silicon wafer from alcoholic sus- a wave-dispersive analyser WDX system Microspec - pension. 3PC. 78 Journal of the Czech Geological Society, 42/4 (1997) For quantitative chemical analysis of mineral phases Crystal data and structure refinement for MOASO in the system Ca-Cu-UO2-CO3-H2O the following condi- Diffractometer Enraf-Nonius CAD4-MACHIII tions were used: the standards: azurite (Cu, C, O), calcite Empirical formula H6 As2 Mo2 O12 Formula weight 539.77 (Ca, C, O), uranium (U). Operating voltage and sample Temperature [K] 293(2) current 20 kV and 40 nA respectively. Specimen beam Wavelength [Å] 0.71069 size was 15u10 Pm. Crystal system Monoclinic For quantitative chemical analysis of MOASO the Space group P21/c following conditions were used: the standards: arsenolite (As, O), molybdenum (Mo). Operating voltage and sam- Unit cell dimensions ple current 20 kV and 20 nA respectively. Specimen a [Å] 7.0398(4) beam size was 5u5 Pm. b [Å] 12.0682(13) Correction procedures ZAF, Phi(rhouZ), and Quadri- c [Å] 12.210(2) E [°] 101.265(9) lateral were used for calculation of all quantitative analy- Volume [Å3] 1017.4(2) ses. Z 4 TG, DTG curves were recorded simultaneously on Density (calculated) [g.cm-3] 3.524 the thermobalance TG 750 Stanton Redcroft. The operat- Absorption coefficient [mm-1] 8.98 F(000) 1008 ing conditions: sample weight about 1-3 mg, heating rate 3 -1 -1 Crystal size [mm ] 0.10 u 0.14 u 0.39 10 qC.min , dynamic air atmosphere 10 ml.min and Theta range for data collection 2.40 to 24.99 temperature range 20-1000 qC. [°4@ Infrared absorption spectra in the 400-4000 cm-1 range were recorded with and FTIR spectrometer Nicolet Index ranges 740 using KBr pellets and/or diffusion reflection mode. h 0; 8 k 0; 14 l -14; 14 New naturally occurring phases Reflections collected 1935 Independent reflections 1787 [R(int) = 0.0489] 2 6+ 3+ Refinement method Full-matrix least-squares on F The phase: [(Mo O2)2As 2O5(H2O)2] . H2O Data / restraints / parameters 1786 / 0 / 145 (MOASO) GOF 1.07 Final R indices [I>2V(I)] R1 = 0.0455, wR2 = 0.1143 It forms minute green to grey-green acicular crystals R indices (all data) R1 = 0.0580, wR2 = 0.1243 '/V (max) 1.745 or continuous crusts, which rim strongly corroded vein- -3 let. Laterally it gives way to grey-green scorodite in '(U) [e.A ] -1.728 spherical and botryoidal aggregates. Sample number: J- R1 =6««Fo ««Fc ««6«Fo «« 2 2 2 2 2 0.5 wR2 = {6>w(Fo -Fc ) ] / 6[w(Fo ) ]} 230. 2 2 2 0.5 The phase was observed on fractures in proximity to GOF = {6>w(Fo -Fc ) ]/(N - P)` strongly weathered arsenopyrite (löllingite)-pyrite vein approximately 5 cm thick, with the sulphides partly or Atomic coordinates ( u 104) and equivalent isotropic displacement 2 3 completely altered to mixture of compact grey-black parameters [Å u 10 ] for MOASO. Ueq is defined as one third of the scorodite with a metallic lustre and arsenolite. Paragene- trace of the orthogonalized Uij tensor. sis: scorodite, parascorodite, arsenolite. x y z Ueq The specimens were collected in the Geschieber vein. Mo(1) 6214(1) 2121(1) 2757(1) 12(1) The phase was formed in highly acid environment of Mo(2) 1799(1) 2321(1) 905(1) 13(1) concentrated sulphuric acid, in the presence of As2O3 in As(3) 2066(1) 1418(1) -1626(1) 13(1) significant concentrations. As(4) 6245(1) 3440(1) 5030(1) 13(1) O(1) -333(9) 2915(5) 1068(5) 24(2) O(2) 4963(8) 1976(5) 1095(4) 14(1) O(3) 1387(10) 951(5) 1006(5) 26(2) O(4) 8084(9) 1267(5) 2671(5) 22(1) Thermogravimetric (TG, DTG) curves of MOASO from Jáchymov O(5) 7186(9) 3414(5) 2745(5) 22(1) O(6) 3147(8) 2659(5) 2485(4) 14(1) O(7) 1681(9) 2432(5) -668(5) 19(1) O(8) 4275(8) 840(5) -875(4) 14(1) O(9) 6029(9) 2158(5) 4300(5) 18(1) O(10) 4588(9) 470(5) 2832(5) 22(1) O(11) 2886(11) 4090(6) 742(6) 34(2) O(12W) 1477(9) 137(6) 3705(5) 25(2) No mineral containing Mo was found in the assem- blage. It is suggested that amorphous, finely dispersed Mo sulphides (jordisite) or oxides, soluble in the acid solutions, served as a source of Mo. The solutions carry- ing Mo6+ probably attained elevated concentrations which resulted in crystallisation of the new phase. Journal of the Czech Geological Society, 42/4 (1997) 79 The quantitative chemical analysis: Mo 35.04, As Details on the structure are given in tables. Basic mo- 27.83, O 36.91 wt. % gives after recalculation based on tif of the structure and projections of it onto ac and bc 12 oxygen atoms the following empirical formula: planes are presented in figures. (MoO2)1.93(As2O5)0.95(OH)0.07 . 3.31 H2O Projection of MOASO crystal structure onto ac plane. c or a simplified formula: (MoO2)2As2O5 . 3 H2O The crystal structure of MOASO was solved from single-crystal data (for details see Experimental met- hods at the beginning of this paper). Polyhedral volumes and deformations expressed as bond angle variance, and quadratic elongation for two [MoO6] octahedra in the crystal structure of MOASO Mo1 Mo2 3 VO [Å ] 9.815 9.736 V2 129.738 121.352 a Q.E.
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