SPECTRO XRF Report SPECTRO XEPOS. Analysis of Raw Material prepared as Fused Bead in the Cement Industry. Summary

Transcription

1 Nr. XRF-43 SPECTRO XEPOS Summary The SPECTRO XEPOS simultaneous XRF spectrometer provides a fast, reliable and economic solution to analyze raw material fused bead for the cement industry. Analysis of Raw in the Cement Industry SPECTRO Analytical Instruments, Kleve 1. Introduction X-ray Fluorescence is a well established technique for analyzing cement and other materials in the cement making process. The performance requirements for analyzing cement are described in various documents. The report describes the calibration and validation of the SPECTRO XEPOS for the simultaneous analysis of the 13 oxides SiO 2, Al 2 O 3, Fe 2 O 3, CaO, MgO, P 2 O 5, SO 3, K 2 O, Na 2 O, TiO 2, Mn 2 O 3, and SrO in cement fused bead. Page 1/6

2 2. Instrumentation SPECTRO XEPOS The measurements were made using a XEPOS XRF spectrometer. The samples were excited for 660 s by forced air cooled 50 W Pd end window X-ray tube combined with the excitation conditions listed in table 1. Table 1: Measurement conditions (Measurement time = clock time, live time is about 50% shorter than given measurement time) Elements kv/ma Target Meas. Time / [s] Na Cl 17.5 kv, 2.0 ma HOPG 300 K Mn 35 kv, 1.0 ma Co 300 Fe Sr 40 kv, 0.88 ma Mo 60 A VITUS-SDD Detector was used to collect the fluorescence radiation from the sample. The spectral resolution of this detector was <160 ev for Mn K α. During the measurement the sample chamber was flushed with He. All measurement parameters are controlled by the system PC. 3. Sample Preparation The samples were fused beads by Fluxana. For the preparation of the fused beads the material was ignited and the loss on ignition was determined. 1 g of the ignited material was mixed with 8 g of Lithiumtetraborat flux and fused to a bead with 40 mm diameter in an automatic fluxer. 4. Calibration and Validation Samples For calibration the samples CEM01, CEM02, CEM03, CEM04, CEM05a, CEM06, CEM07, CEM08, CEM09, CEM10a, CEM11, and RAW 1- RAW 13 from Fluxana were used. The calibration was validated with various international reference samples from JIS 1, NIST 2, BCS 3, GBW 4, BAS 5, Dillinger Huette, Domtar. The samples were: BCS 394: bauxite JIS 13 : cement JIS 3 : cement NIST 1413 : sand, high alumina Dillinger Huette SX 09-07: dolomite Domtar GYP C: gypsum BAS 683-1: Iron ore sinter NIST 698: bauxite, jamaican GBW : rock GBW : limestone 5. Calibration The calibrations were performed by measuring a set of samples listed in section 4. based on a fundamental parameters method for matrix correction purposes. The concentration ranges, the RMS-error of calibration. RMS = n ( Ccertified Ccalculated ) i=1 n f and the correlation coefficients, r, are given in Table 2. 1 JIS: Japanese Industrial Standard 2 National Institute of Standards & Technology 3 British Chemical Standard 4 National Research Center for Reference s, China 5 Bureau of Analyzed Samples 2 Page 2/6

3 Table 2: Calibration ranges, root mean square error of calibration and correlation coefficients for 14 components in cement Range % RMS SiO Al 2O Fe 2O CaO MgO P 2O SO K 2O Na 2O TiO Mn 2O Line overlap and matrix corrections were applied where necessary. The low RMS errors are caused by the excellent sensitivities of the SPECTRO XEPOS for the given elements (oxides). The following graphs show as examples the correlation for SiO 2 and Al 2 O 3. calculated in % R 2 = 0, Fig 1: Correlation plot for SiO 2 given in % % r calculated in % Fig 2: Correlation plot for Al 2O 3 6. Validation After the calibration various samples were run for validation. The analysis results of these samples versus the certified values are listed in the following tables. For all samples the results were calculated back to the original substance with consideration of the given loss on ignition (LOI). Table 3: Analysis results versus certified values for validation sample BCS 394 bauxite (LOI: 0.4 %) R 2 = 0, given in % SiO ± 0.01 Al 2O ± 0.07 CaO ± 0.01 MgO 0.12 < 0.1 P 2O ± 0.01 SO ± 0.01 K 2O ± 0.01 Na 2O 0.02 < 0.1 TiO ± 0.01 Mn 2O ± SrO ± Page 3/6

4 Table 4: Analysis results versus certified values for validation sample JIS 13 cement SiO ± ± 0.02 Al 2O ± ± 0.02 Fe 2O ± ± 0.01 CaO ± ± 0.04 MgO 3.03 ± ± 0.02 P 2O ± ± SO 3 2,00 ± ± 0.01 K 2O 0.38 ± ± 0.01 Na 2O 0.39 ± ± 0.02 TiO ± ± Mn 2O ± ± 0.01 SrO ± ± Table 6: Analysis results versus certified values for validation sample NIST 1413 sand high alumina SiO ± ± 0.05 Al 2O ± ± 0.03 Fe 2O ± ± 0.01 CaO 0.74 ± ± 0.01 MgO 0.06 ± ± 0.01 P 2O ± 0.01 SO ± 0.01 K 2O 3,94 ± ± 0.01 Na 2O 1.75 ± ± 0.04 TiO ± ± 0.01 Mn 2O ± SrO ± Table 5: Analysis results versus certified values for validation sample JIS 3 cement SiO ± ± 0.02 Al 2O ± ± 0.02 Fe 2O ± ± 0.02 CaO ± ± 0.04 MgO 1.53 ± ± 0.02 P 2O ± ± SO ± ± 0.01 K 2O ± ± 0.01 Na 2O ± ± 0.01 TiO ± ± Mn 2O ± ± SrO ± ± Table 7: Analysis results versus certified values for validation sample SX09-07 dolomite (LOI 44.68%) SiO ± ± 0.01 Al 2O ± ± Fe 2O ± ± 0.01 CaO ± ± 0.02 MgO ± ± 0.04 P 2O ± ± SO ± ± K 2O ± ± 0.01 Na 2O ± < 0.1 TiO ± ± Mn 2O ± ± SrO ± Page 4/6

5 Table 8: Analysis results versus certified values for validation sample Domtar GYP C gypsum (LOI 25.93%) SiO ± 0.01 Al 2O ± 0.01 Fe 2O ± 0.01 CaO ± 0.02 MgO ± 0.03 P 2O ±0.001 SO ± 0.03 K 2O ± 0.01 Na 2O ± 0.01 TiO ± Mn 2O ± SrO ± 0.01 Table 10: Analysis results versus certified values for validation sample NIST 698 bauxite (LOI 27.3 %) SiO ± ± 0.01 Al 2O ± ± 0.04 Fe 2O ± ± 0.04 CaO 0.62 ± ± 0.01 MgO 0.06 ± ± 0.01 P 2O ± ± 0.01 SO ± K 2O ± ± 0.01 Na 2O ± 0.02 TiO ± ± 0.01 Mn 2O ± ± SrO ± Table 9: Analysis results versus certified values for validation sample BAS iron ore sinter SiO ± ± 0.02 Al 2O ± ± 0.01 Fe 2O ± ± 0.12 CaO 7.89 ± ± 0.01 MgO 1.70 ± ± 0.02 P 2O ± ± SO ± K 2O ± ± 0.01 Na 2O 0.06 ± ± 0.02 TiO ± ± 0.01 Mn 2O ± ± SrO ± Table 11: Analysis results versus certified values for validation sample GBW limestone (LOI 34.1 %) SiO ± ± 0.02 Al 2O ± ± 0.02 Fe 2O ± ± 0.01 CaO ± ± 0.03 MgO 5.19 ± ± 0.02 P 2O ± ± SO ± K 2O 0.78 ± ± 0.01 Na 2O ± 0.01 TiO ± ± Mn 2O ± ± SrO ± ± Page 5/6

6 Table 12: Analysis results versus certified values for validation sample GBW limestone (LOI %) SiO ± ± 0.01 Al 2O ± ± 0.01 Fe 2O ± ± 0.01 CaO ± 0.03 MgO 3.63 ± ± 0.02 P 2O ± ± SO ± K 2O 0.23 ± ± 0.01 Na 2O ± ± 0.01 TiO ± ± Mn 2O ± ± SrO ± Summary All results show that SPECTRO XEPOS is capable to analyze raw material for the cement industry fused beads with superb accuracy. The calibrations show low values for RMS and high correlation coefficients. The results of the validation samples show an excellent agreement between expected and analyzed concentrations. In view of size, performance and cost of ownership the SPECTRO XEPOS meets also the requirement of modern laboratories. GERMANY SPECTRO Analytical Instruments GmbH Boschstrasse 10 D Kleve Tel: Fax: spectro.info@ametek.com U.S.A. SPECTRO Analytical Instruments Inc. 91 McKee Drive Mahwah, NJ Tel: Fax: spectro-usa.info@ametek.com HONG KONG (Asia-Pacific) SPECTRO Analytical Instruments (Asia-Pacific) Ltd Sino Favour Centre 1 On Yip Street Chaiwan Tel: Fax: spectro-ap.info@ametek.com Subsidiaries: CHINA: Tel , Fax , spectro-china.info@ametek.com.cn, FRANCE: Tel , Fax , spectro-france.info@ametek.com, GREAT BRITAIN: Tel , Fax , spectro-uk.info@ametek.com, ITALY: Tel: , Fax , spectro-italy.info@ametek.com, JAPAN: Tel: +81-(0) , Fax: +81-(0) , spectro-japan.info@ametek.com, SWEDEN: Tel: , Fax: , spectro-nordic.info@ametek.com, SOUTH AFRICA: Tel , Fax , spectro-za.info@ametek.com. SPECTRO operates worldwide and is present in more than 50 countries. Please contact our headquarters for your local representative. Page 6/6 SPECTRO 2008, Subject to modifications B-08, Photos: SPECTRO.