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  • Rapid Determination of CaO and SO3 in Loose-Powder Cement by Energy

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    jorgehrdz269
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    Análisis químicos para la determinación de de Oxido de Calcio y Sulfito en cemento

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    Análisis químicos para la determinación de de Oxido de Calcio y Sulfito en cemento

    Drepturi de autor:

    © All Rights Reserved
    Descărcați ca PDF sau citiți online pe Scribd
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    10 vizualizări6 pagini

    Rapid Determination of CaO and SO3 in Loose-Powder Cement by Energy

    Încărcat de

    jorgehrdz269
    Análisis químicos para la determinación de de Oxido de Calcio y Sulfito en cemento

    Drepturi de autor:

    © All Rights Reserved
    Descărcați ca PDF sau citiți online pe Scribd
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    din 6
    INDUSTRIAL CHEMISTRY RESEARCH COMMUNICATIONS 1(4): 41 -46 (2005) RAPID DETERMINATION OF CaO AND SO, IN LOOSE-POWDER CEMENT BY ENERGY DISPERSIVE X-RAY FLUORESCENCE (EDXRF) TECHNIQUE S. A. Adebayo', L. G. Mustapha! and S. A. Kareem'? | ABSTRACT: Percentage CaO and SO, contents in loose-powder cement were rapidly determined using | EDXRF spectrometry. To avoid the absorption of secondary x-rays from the low-atomic number elements (Ca and S), measurements were carried out in a helium atmosphere instead of in air. Sampie pasticle size was further reduced by grinding in a rotating-disc gyratory mill for a period of 120 seconds. The results show a high degree of accuracy and precision technically desired for process control in a cement factory. The method was found to be more efficient (less time-consuming and more cost-saving) compared to the Pressed pellet rte fused-bead methods employed in the EDXRF spectrometric andthe spectrophatometrc | and gravimetric methods often used in industry. L.INTRODUCTION: Stringent quality requirements are imposed on the production of cement to ensure that the correct mechanical strength is achieved after setting. Obviously, it is impracticable in production control to monitor this directly since the complex hydration process can take months, and the full strength is not reached until it is complete (Field, 1988). CaO and SO, have been found to have significant effects con the strength development of cement (Taylor, 1964). There is an optimum SO, level for good strength development (Meissner, 1950), Effective monitoring of these compounds during production is therefore required to ensure that cement with the right strength development is produced. Spectrophotometric, gravimetric and other wet analytical methods have been employed over the years for the determination of CaO and SO, in cement (British Standards Institution, 1970). However, the desire to | obtain resuits within a short time and at lower cost, with ease of analysis required for effective quality | control, has led to the development of other rapid methods of analysis (Abdulrahman, 1987; Maruta et al, 199.3). Kray fluorescence (XRF) analysis has been in use in the cement industry for over four decades for the determination of basic oxides in cement and cement raw materials (Robson, 1991). XRF analysis has shown itself to be a faster, more reliable, simpler and more accurate method of analysis than other methods of analysis (Price and Platt, 1990). “The fusion of samples into beads (prepared by taking 1 part by weight of sample with five parts by weight | of flux and fusing at 1200°C) and pressing into pellets in XRF analysis sample preparations is to overcome | 1. Departaead of Chemistry, University of Horin, Horin, Nigeria 2. Author to whom correspondence should be addressed. (al “© 2005. Research Communications, Lagos, Nigeria. ISSN 1595-0964 oo Determination of C20 and SO, in Loc “Powder Cement by EDRF particle size variations. Variations in particle size will give differing secondary x-ray intensities and, hence, | variations in results, In such cases, sample preparation takes a longer time and is less economical | In the method described in this report, sample preparation time is greatly reduced while atthe same time ) | particle size variation is minimized, by grinding samples into loose powder, such that accurate and reproducible | | results are obtained at a much shorter time and at lesser cost. | 2. MATERIALS AND METHODS: Clinker and gypsum samples were obtained from the Ewekoro | Works of the West African Portland Cement Company (WAPCO) Plc. The samples were collected using standard sampling methods (Standards Organisation of Nigeria, 1995). Standard cement samples were prepared by grinding cement clinker and gypsum together in a laboratory scale ball mill. Percentage CaO | and SO, were varied by varying the percentage of gypsum added. | CaO and $O, in the standard samples were determined by standard wet methods (Standards Organisation | of Nigeria, 1995). The standards have a concentration range encompassing the range of interest for | | normal routine measurements. | | Using the Oxford Lab-X%° XRF spectrometer, a spectrum scan of the standards was carried out to | ensure correct measurement conditions. The spectrometer was calibrated with the standards | To overcome problems of particle size variation, 20g of loose- powder cement further pulverised in a | gyratory disc mill for 120. seconds. The fine-powder cement sample was poured into a sample cup fitted | with a 6um thick polycarbonate film as the window material. The cup was gently tapped to ensure the | sample in the cup has a flat surface. It was then placed in the sample port of the x-ray spectrometer, and CaO and SO, were measured over 100 seconds against the prepared calibration (which relates the intensities of the elemental spectra-lines and concentration), | Helium gas at a flow rate of 1.7L/min and a pressure of | bar was used to flush the air between the detector and the sample for optimum analytical performance. 3. RESULTS AND DISCUSSION: Figure 1 shows the change in intensity (counts per second, CPS) against grinding time.CaO has a higher optimum grinding time than SO,. The optimum grinding time for | CaO is 120 seconds as against 30 seconds for SO,. According to Robson (1991), an optismum time is | chosen which is the best for the most important element. The optimum time is the time corresponding to | the maximum intensity peak for the mest important element,CaO being the most abundant and, hence, | most important component of cement, its grinding time of 120 seconds corresponding to the peak intensity A C ‘Adebayo, Montapha & Kareom Indust, Chem. Rex. Comm. 1(4): 39 - #4 005) was used as the optimum grinding time for analysis. ‘The spectrum scan of loose-powder cement (for both CaO and SO,) used to identify the channel number(s) required for calibration on the spectrometer is shown in Figure 2. The calcium signals dominate the spectrum because of the abundance of CaO in ordinary Portland cement ( OPC), usually in the range of 60 to 64%, and SO,, usually <=3%, This is in agreement with the report of Oxford Instruments Industrial Analysis Group (1993) which shows that when a cement sample is excited by a radioactive source, the calcium x-rays dominate the epectrum making it difficult to measure the much weaker sulfur signals. The channel number for CaO is between 40 and 70 with the peak at 60. SO, has a channel number between 80 and 110 with the peak at 90. The calibration for both CaO and SO, has a linear relationship between concentration ‘Table I shows the results of measurements of CaO and SO, in cement using wet, fused-bead, pressed- pellet and loose-powder methods, Each result is the mean of three measurements for each of the samples. CaO and my Loose-Powsder * Pressed-Pellet Fused-Bead ‘Wet x0 SO, C0 $0, cao | so, | CO] SO, (%) (%) (%) (%) (%) (%) (%) (%) A | 6105 253 105 “254 | 6106 254 | 6107 254 B | 6237 22 e240 20 | 6239 210 | 6239 2 Cc | was 200 349 202 | 6346 201 | 63.48 201 D | as 192 83 189 | 55 19 | 6.56 1st E | 6.65 we 63.62 176 | 6359 179 | 63.60 176 |] F | 610s LD 10 110 | 64.05 qs | 6405 ua | From the Table, the results by the loose-powder, pressed-pellet, fused-bead and wet methods are quite in agreement. This shows that any of the four methods could be used for monitoring CaO and SO, in cement. However, the wet method is time-consuming, taking at least four hours for completion. This is in | asicement with he Sindins of Abdurahman (1987). In he cement industry, this method may not be good enough for effective quality control. The fused~bead and the pressed-pellet methods are faster than the | wet method but much costlier, requiring additional equipment (press mill, Claisse fuxy fusion machine), The loose-powder method is however easier, faster and less costly than the other three, thus facilitating | effective monitoring of production as more samples can be analysed more frequently, A maximum Lo {a3} I Determination of C40 and SO, in Loose Powder Cement by EDXRF 6 Uptimum grinding time for Cao and say ‘ing tn) ‘Spectrum Scah of, loose powder cement. 1iss rs nn ae

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