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Quantitative Analysis of Mineralized White

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Quantitative Analysis of Mineralized White Quantitative analysis of mineralized white Portland clinkers: The structure of Fluorellestadite Isabel Pajares Instituto de Ciencias de la Construccio´n ‘‘Eduardo Torroja,’’ CSIC, C/Serrano Galvache s/n, 28033-Madrid, Spain A´ ngeles G. De la Torre Departamento de Quı´mica Inorga´nica, Cristalografı´a y Mineralogı´a, Universidad de Ma´laga, 29071-Ma´laga, Spain Sagrario Martı´nez-Ramı´rez, Francisca Puertas, and Marı´a-Teresa Blanco-Varela Instituto de Ciencias de la Construccio´n ‘‘Eduardo Torroja,’’ CSIC, C/Serrano Galvache s/n, 28033-Madrid, Spain Miguel A. G. Arandaa) Departamento de Quı´mica Inorga´nica, Cristalografı´a y Mineralogı´a, Universidad de Ma´laga, 29071-Ma´laga, Spain ͑Received 1 April 2002; accepted 15 July 2002͒ Fluorellestadite, Ca10(SiO4)3(SO4)3F2 , has been synthesized as single phase. This compound ϭ crystallizes in the apatite type structure, s.g. P63 /m, with parameters a 9.4417(1) Å, c ϭ ϭ 3 6.9396(1) Å and V 535.76(1) Å . The refinement of its crystal structure converged to RWP ϭ ϭ 12.33% and RF 4.58%. The atomic parameters have been used to analyze the phase content of mineralized white Portland clinkers. These clinkers contain Ca3SiO5 ,Ca2SiO4 ,Ca12Al14O32F2 and Ca10(SiO4)3(SO4)3F2 . The agreement between the elemental composition inferred from the Rietveld phase analysis and that measured by XRF is noteworthy. This comparison does not take into account the presence of amorphous phases and unmodeled elemental substitutions in crystalline phases. Similar Rietveld studies on commercial white Portland clinkers are also shown to be feasible. © 2002 International Centre for Diffraction Data. ͓DOI: 10.1154/1.1505045͔ INTRODUCTION below 1200 °C ͑Gime´nez and Blanco-Varela, 1995; Blanco- Varela et al., 1986͒. For the production of Portland clinkers, mineralizers It is of great importance to know the mineralogical com- and/or fluxes are often added to the raw mixes to accelerate positions of these clinkers in order to understand and predict reactions and enhance burnability. Traditional fluxes such as the mechanical strength of mortars or concrete elaborated Fe2O3 and Al2O3 have been partially substituted by the min- with these cements. So far, calculations with the method of eralizing pair CaF2 /CaSO4 to produce clinkers with low alu- Bogue ͑1929͒ are used to deduce the mineralogical compo- minate contents at temperatures between 1300 and 1400 °C sition by using the elemental content usually measured by ͑Gime´nez et al., 1991; Blanco-Varela et al., 1985, 1990; X-Ray Fluorescence ͑XRF͒. This method has well known Moir, 1982; Blanco-Varela et al., 1997; Wenxi et al., 1992͒. problems ͑Taylor, 1997͒ mainly due to the lack of thermody- The use of this mineralizing pair to partially replace alumi- namical equilibrium in the kiln. Hence, alternative analytical nates is particularly useful in manufacturing white clinkers, methods are being studied to measure the mineralogical because of the potential for energy conservation and seawa- compositions of clinkers and cements. Laboratory X-Ray ter resistance ͑Pajares et al., 2001͒. Powder Diffraction, LXRPD, is now widely used to carry out The phases that may be present in this type of mineral- quantitative phase analyses of crystalline mixtures ͑Hill and ized clinkers ͑Gime´nez and Blanco-Varela, 1995͒ are: alite, Howard, 1987; Bish and Howard, 1988; Madsen et al., 2001͒ ͓C3S, Ca3SiO5]; belite, ͓C2S, Ca2SiO4]; calcium aluminate by using the Rietveld method ͑Rietveld, 1969; McCusker ͓C12A7 ,Ca12Al14O33] or a related compound ͓C11A7CaF2 , et al., 1999͒. The method compares the measured pattern and ͓ Ca12Al14O32F2]; and fluorellestadite 6CaO•3SiO2 that calculated with the crystal structures. This methodology ͑ •3CaSO4•CaF2 or Ca10(SiO4)3(SO4)3F2]. The alite rate for- has recently been applied to Portland clinkers De la Torre mation, in the presence of the mineralizing pair et al., 2001͒, aluminous cements ͑Guirado et al., 2000͒ and (CaF2 /CaSO4) is higher than that found for mixes mineral- calcium sulpho-aluminate cements ͑Schmidt and Po¨llmann, ͑ ͒ ized only with CaF2 Christensen and Johansen, 1980 . This 2000͒. The interest on the application of XRD to Portland ͑ faster rate for C3S is mainly due to the thermodynamic effect cements is recently increasing Goswami and Panda, 1999; of widening its stability range and the primary phase field of Taylor et al., 2000͒. crystallization. Additionally, ion mobility in the melt is en- On the other hand, in order to apply the Rietveld method hanced by CaSO4 and CaF2 as a new liquid phase appears to mineralized clinkers it is necessary to know the structure of fluorellestadite. Unfortunately, the crystal structure of this phase was not known although it can be prepared as a crys- a͒ Author to whom correspondence should be addressed: Departamento de Quı´mica Inorga´nica, Cristalografı´a y Mineralogı´a, Universidad de Ma´laga, talline single phase. Its powder pattern is present in the PDF ͑ ͒ 29071-Ma´laga, Spain, Phone: Intϩ34 952131874, Fax: Int Database JCPDS-ICDD with a hexagonal cell, s.g. P63 /m, ϩ ϭ ϭ ͑ 34 952132000, electronic mail: g–[email protected] of a 9.441 Å and c 6.939 Å Po¨llman and Neubauer, 281 Powder Diffraction 17 (4), December 2002 0885-7156/2002/17(4)/281/6/$18.00 © 2002 JCPDS-ICDD 281 TABLE I. Chemical analysis for the raw materials and mineralized clinker ͑%w/w͒. Sample Sand Limestone Kaolin Fluorite Gypsum Clinker-ECa Clinker-EAb Clinker-PAc SiO2 89.43 3.79 57.72 - 1.68 23.04 22.25 26.2 Al2O3 5.11 0.75 27.94 - 0.00 2.61 2.70 1.05 Fe2O3 0.22 0.32 0.60 - 0.10 0.45 0.34 - CaO 1.46 53.76 1.12 - 37.86 67.73 69.06 69.3 MgO 0.42 0.35 0.98 - 0.07 0.53 0.88 - SO3 0.00 0.00 0.00 - 40.05 2.75 2.98 2.50 K2O 0.93 0.11 0.23 - 0.05 0.32 nd - Na2O 0.11 0.22 0.11 - 0.08 0.29 nd - CaF2 - - - 99.9 - 2.28 nd 0.95 Lossd 2.30 40.70 11.29 - 20.11 - 0.48 - Ratioe 12.45 79.72 1.76 1.51 4.56 - - - a Expected composition for the mineralized clinker taking into account the raw materials ratio. b Elemental analysis of the mineralized clinker by XRF and expressed as oxide content. c Phase analysis of the mineralized clinker by the Rietveld method and expressed as oxide content. d Weight loss by heating at 1000 °C. e Raw materials ratio for the preparation of the mineralized clinker. 1993͒. The structure must be similar to that of apatite where White Portland clinker the phosphate groups are randomly replaced by silicate and A typical commercial white Portland clinker was sulphate tetrahedra and the hydroxyl groups are replaced by sampled from a factory and characterized by powder diffrac- ͓ the fluoride anions. In fact, a structure for ellestadite ap- tion. proximately Ca10(SiO4)3(SO4)3(OH)2] has been reported for a mineral from Cuba ͑Organova et al., 1994͒. This crystal was monoclinic but with the apatite framework and it con- LXRPD studies tained chloride anions and even a small amount of carbonate. The LXRPD pattern for FLELL was recorded on a The aim of this work is to determine the crystal structure Siemens D5000 ␪/2␪ diffractometer ͑flat reflection mode͒ by of fluorellestadite and use it for the quantitative analysis of ␣ ͑ ͒ using CuK 1,2 radiation 1.542 Å with a secondary curved the mineralized white Portland clinkers. graphite monochromator at 25 °C. The samples were loaded in an aluminum holder by sample-front pressing. The experi- mental details are given in Table II. The LXRPD data for a EXPERIMENT commercial white Portland clinker were collected as for the Fluorellestadite synthesis mineralized clinker but spinning the sample at 15 rpm to The raw materials used for fluorellestadite, FLELL, improve the particles statistics. (6CaO•3SiO2•3CaSO4•CaF2) synthesis were CaCO3 , CaSO4•2H2O, SiO2 and CaF2 with high purity grade in the stoichiometric ratio. The ground mixture was heated at RESULTS AND DISCUSSION 1000 °C for 2 h. Then, the sample was ground again in an The final goal of this work is the determination of the agate mortar and heated at 1000 °C for 32 h. To follow the mineralogical composition of mineralized white Portland synthetic procedure, free lime concentration was determined clinker by powder diffraction using the Rietveld methodol- by the ethylene-glycol method ͑UNE Standard 80-243-86, ogy. However, to do so, the structural information of all crys- 1986͒ giving 0.42% w/w of CaO. Routine LXRPD data in- talline phases is needed. As the crystal structure of FLELL dicated that the sample was a highly crystalline single phase. was not known, this structure was determined prior to the mineralogical quantification. Mineralized white Portland clinker preparation The chemical analysis of the raw materials used for the Crystal structure of Fluorellestadite preparation of the mineralized clinker is presented in Table I. FLELL crystallizes in an hexagonal cell, s.g. P63 /m, In order to get the required mineralizers content, the dosage PDF no. 45-0009, with edges very similar to those of the given at the bottom of Table I was selected. The resulting apatite type structure. Hence, the fluorapatite structure has silica modulus was 7.50 ͑% w/w͒. The raw materials were been used as starting model ͑Mackie and Young, 1973͒. The ground to particle size smaller than 45 ␮m except limestone powder pattern was analyzed by the Rietveld method with which was ground to particle size smaller than 125 ␮m.
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