ANALYSIS OF MAJOR AND

MINOR ELEMENTS IN BAUXITE

SAMPLES PREPARED AS
FUSED BEADS
Introduction
In order to perform the right quality control of bauxite raw material,
not only the aluminium concentration is monitored, but also
concentrations of other elements like silicon (Si), iron (Fe) and
titanium (Ti), which are of vital importance.
This application note describes the analysis of major and minor
elements present in bauxite prepared as fused beads, using
the Epsilon 4 energy dispersive X-ray fluorescence (EDXRF)
spectrometer together with the Claisse Eagon 2 fusion machine.
Sample preparation
Calibrations were set up using seven certified reference materials
(CRM) prepared in duplicates as fused beads. The CRMs include
NIST (696b, 600, 696, 697) and GBW (07177, 07181, 07182). The
fused beads were prepared using a 1/10 flux (50% Li2B4O7/50%
LiBO2) to sample ratio. The fusions were performed at 1150°C
using a Claisse Eagon 2 automatic fusion machine.
Instrumentation
Measurements were performed using the Epsilon 4 EDXRF
spectrometer, equipped with a 10 W, 50 kV silver anode X-ray
tube, 6 filters, a helium purge facility, a high-resolution silicon drift
detector (SDD), a sample spinner and a 10-position removable
sample tray.
Measurement conditions
The measurement conditions for measuring Al2O3, CaO, Cr2O3,
Fe2O3, K2O, MgO, MnO, P2O5, SO3, SiO2, TiO2, ZnO and ZrO2
present in the prepared samples are given in Table 1. The total
measurement time per sample was 4 minutes.
Figure 1 shows the spectra for Al2O3 and SiO2 of a NIST bauxite
standard.

Table 1. Measurement conditions

Compounds kV µA Measurement Medium Filter
time (s)
Al2O3, MgO, P2O5, SO3, SiO2 5 2000 60 Helium None
CaO, Cr2O3, Fe2O3, K2O, MnO, TiO2 12 800 120 Air A-thin
ZnO, ZrO2 50 200 60 Air Ag

Accurate calibration results

The calibration graphs for Al2O3, Fe2O3 and TiO2 in fused bauxite
are shown in Figures 2, 3 and 4, respectively, demonstrating the
good correlation between the certified concentrations and the
measured intensities. Table 2 lists the root mean square (RMS)
of the individual compound calibrations. The LLD values are
calculated using the measurement times documented in Table 1.

Precise results
A repeatability test was performed by measuring NIST 698
standard twenty times, to test the precision of the Epsilon 4. The
results are given in Table 3.

The results show a good agreement between certified and

average measured concentrations. The low RMS values for the
Figure 1. The spectrum of standard NIST 696B, obtained with 5 kV under repeatability measurements show the good stability of the system
helium; showing the excellent resolution and the high sensitivity of the as a whole.
detector
 Table 2. Calibration results

Compound Concentration Calibration LLD (ppm)

range (wt%) RMS* (wt%) application time
Corrected intensity

Al2O3 40.0 - 90.63 0.363 n.a.

CaO 0.018 - 0.71 0.020 33
Cr2O3 0.011 - 0.100 0.003 21
Fe2O3 1.24 - 20.0 0.069 n.a.
K2O 0.009 - 0.23 0.005 34
MgO 0.012 - 0.18 0.036 120
MnO 0.003 - 0.41 0.005 14
P2O5 0.039 - 0.97 0.068 95
42 48 54 60 66 72 78 84 90 SO2 0.077 - 0.551 0.017 35
Al2O3 concentration (wt%) SiO2 0.69 - 20.3 0.138 n.a.
Figure 2. Calibration graph for Al2O3 in bauxite TiO2 1.31 - 3.8 0.040 n.a.
ZnO 0.001 - 0.037 0.001 14
ZrO2 0.060 - 0.29 0.009 19
* RMS (root mean square) value is an indication of the quality of the regression. The more accurate
calibrations have the smaller RMS values.
Corrected intensity

of this information and we shall not be liable for errors contained herein or for damages in connection with the use of this material. Malvern Panalytical reserves the right to change the content in this material at any time without notice.
Table 3. Results of the repeatability test

Disclaimer: Although diligent care has been used to ensure that the information in this material is accurate, nothing herein can be construed to imply any representation or warranty as to the accuracy, correctness or completeness
NIST 698 Certified Average measured RMS
(n = 20) concentration concentration (wt%)
(wt%) (wt%)
Al2O3 48.2 48.04 0.04
CaO 0.62 0.572 0.003
Cr2O3 0.08 0.076 0.001
Fe2O3 19.6 19.36 0.01
0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0
K2O 0.01 0.015 0.003
Fe2O3 concentration (wt%)
MgO 0.058 0.037 0.003
Figure 3. Calibration graph for Fe2O3 in bauxite
MnO 0.38 0.373 0.002

Copyright: © 2018 Malvern Panalytical. This publication or any portion thereof may not be copied or transmitted without our express written permission. 9498 707 62011 PN11199
P2O5 0.37 0.43 0.01
SO3 0.144 0.139 0.002
SiO2 0.69 0.69 0.01
TiO2 2.38 2.32 0.01
Corrected intensity

ZnO 0.029 0.027 0.001

ZrO2 0.061 0.076 0.001

0.0 1.2 1.5 1.8 2.1 2.4 2.7 3.0 3.3

TiO2 concentration (wt%)

Figure 4. Calibration graph for TiO2 in bauxite

Conclusion: This work clearly demonstrates the suitability of

the Epsilon 4 EDXRF spectrometer for the quantitative analysis
of Al2O3, CaO, Cr2O3, Fe2O3, K2O, MgO, MnO, P2O5, SO3,
SiO2, TiO2, ZnO and ZrO2 in bauxite prepared as fused beads.
Accurate and precise results can be obtained in just 4 minutes.

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