Bruker AXS GmbH

X-Flash detector
S2 RANGER

Limestone
deposit

Pressed pellets

Lab Report XRF # 82

S2 RANGER
Fast Analysis of MgO and Main Result

Components in Limestone

This report describes the analytical performance of the Instrumentation

S2 RANGER with XFlash detector for limestone samples,
including the light element magnesium.
Introduction
Like anywhere in the industrial minerals sector, mined raw
material as well as processed limestone must be monitored
on a daily basis in order to ensure constant composition and
quality of the final products.
The S2 RANGER is an all-in-one benchtop energy-dis-
persive X-ray fluorescence (EDXRF) spectrometer with
TouchControl, an easy-to-use touch screen interface. The
system requires only electrical power. Its unique XFlash
detector easily processes input count rates of 100,000 cps
while ensuring excellent resolution, low dead time and high
signal stability. The all-in-one design of the S2 RANGER
includes a vacuum pump in the instruments cabinet, ensur-
ing the best possible performance for this application.

The required precision is on the order of 0.1 wt. % for the

Sample Preparation
MgO content. This is a demanding requirement because
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MgO in limestone produces low fluorescence yield and
heavier elements cause high absorption of X-rays in the
matrix.
Limestone samples were prepared as pressed powder pel-
lets without binding agent. Ten grams of the milled powder
were pressed in aluminum cups (40 mm in diameter) on a
bed of 2.5 g of boric acid while applying a pressure of 8 tons
for 20 s. Such preparation can be performed with any com-
mercially available pellet press.
 Table 1: Measurement conditions Measurement Parameters

Voltage Current Beam Live Time Elements Measurements were performed on an S2 RANGER with
[kV] [A] Filter [s] Analyzed XFlash detector, in vacuum with a 30 mm sample holder
mask. Table 1 lists the measurement conditions used.
20 130 none 100 Mg, Al, Si, Ca,
Mn, Fe
This is a fast method with a measurement time of only 100
seconds and a fixed current of 130 A. These conditions
were selected to take advantage of the excellent resolu-
tion and count rate stability of the XFlash detector. Overall
EDXRF Spectrum detector count rate was well in excess of 100,000 cps. The
overall analysis time (including sample handling, evacuation
of the sample chamber and actual counting time for the
measurement) was 4:20 minutes. Vacuum was below 0.1
mbar for each sample.

Calibration
The excellent energy resolution of the XFlash detector
separated the spectral lines of Al, Si and Mg. Figure 1
shows the low-energy range of the spectrum from a typical
limestone sample.

A set of 12 reference samples was used to set up calibra-

tions for the compounds MgO, Al2O3, SiO2, CaO, Mn3O4 and
Fe2O3. No matrix absorption correction was applied.

Calibration curve in SPECTRA EDX

Figure 1: Spectrum of a typical limestone sample1 including Pd L 1

tube line.

Table 2: Details of calibration data 1

Concentration Calibration
Range standard deviation
[wt. %] 1 [wt. %]
MgO 0.43 1.85 0.1032
Al2O3 0.07 4.65 0.0914
SiO2 0.33 13.30 0.6778
CaO 44.15 55.19 0.5383
Mn3O4 0.015 0.280 0.0048
Fe2O3 0.068 1.000 0.0206

Figure 2: Calibration curve for MgO

1
The given calibration data are typical values and depend
strongly on the reference materials used in the specimen
preparation and on the measurement conditions.

2
Measurement Precision
Measurement of one limestone pellet was repeated 13
times against this calibration. The sample was always
unloaded and reloaded between the measurements. Table
3 demonstrates the impressive stability of the results for
obtained with the S2 RANGER. The required precision of
0.1 wt. % was easily achieved.

Table 3: Precision of the measurement (100 s) of main com-

ponents in limestone

Time MgO Al2O3 SiO2 CaO Mn3O4 Fe2O3

100 s [wt. %] [wt. %] [wt. %] [wt. %] [wt. %] [wt. %]
Rep-1 0.8423 0.4795 1.5988 53.6814 0.0371 0.2547
Rep-2 0.7691 0.4643 1.5956 53.7039 0.0339 0.2536
Rep-3 0.8565 0.4690 1.6013 53.6829 0.0379 0.2571
Rep-4 0.8322 0.4579 1.5827 53.6866 0.0342 0.2491
Rep-5 0.8419 0.4610 1.6084 53.7157 0.0351 0.2517
Rep-6 0.9180 0.4777 1.6202 53.7394 0.0349 0.2526
Rep-7 0.8553 0.4453 1.5973 53.7738 0.0360 0.2613
Rep-8 0.8533 0.4678 1.6026 53.6778 0.0394 0.2601
Rep-9 0.7953 0.4646 1.5887 53.7326 0.0345 0.2601
Rep-10 0.9509 0.4997 1.6049 53.7178 0.0375 0.2592
Rep-11 1.0649 0.4865 1.6136 53.7308 0.0367 0.2591
Rep-12 0.9178 0.4689 1.6006 53.7753 0.0367 0.2578
Rep-13 0.9031 0.4661 1.5924 53.7110 0.0375 0.2570
Average 0.8770 0.4699 1.6005 53.7176 0.0363 0.2564
Abs.Std.Dev. 0.0729 0.0131 0.0096 0.0312 0.0016 0.0036
Rel.Std.Dev. 8.31 2.78 0.60 0.06 4.39 1.41

In order to demonstrate the limits of the EDXRF method, a

repetition test with the same sample was conducted with
an extended measurement time of 1000 s. Table 4 proves
the impressive signal stability of the instrument. In the case
of MgO, the error of measurement was only 0.016 %.

3
Table 4: Precision of main components in limestone with
1000 s measurement time

Time MgO Al2O3 SiO2 CaO Mn3O4 Fe2O3

1000 s [wt. %] [wt. %] [wt. %] [wt. %] [wt. %] [wt. %]
Rep-1 0.8697 0.4650 1.5879 53.5054 0.0368 0.2564
Rep-2 0.8571 0.4710 1.5857 53.4575 0.0377 0.2565
Rep-3 0.8764 0.4725 1.5979 53.5355 0.0371 0.2574
Rep-4 0.8593 0.4686 1.5863 53.5471 0.0365 0.2583
Rep-5 0.8693 0.4755 1.5930 53.5471 0.0369 0.2574
Rep-6 0.8751 0.4709 1.5948 53.5022 0.0376 0.2570
Rep-7 0.8830 0.4729 1.5903 53.5639 0.0378 0.2595
Rep-8 0.8857 0.4728 1.6007 53.5389 0.0368 0.2569
Rep-9 0.8883 0.4700 1.5970 53.5233 0.0369 0.2579
Rep-10 0.9055 0.4726 1.5926 53.5042 0.0373 0.2557
Rep-11 0.9064 0.4728 1.5944 53.4928 0.0363 0.2585
Rep-12 0.8970 0.4703 1.5921 53.4968 0.0364 0.2556
Average 0.8811 0.4712 1.5927 53.5179 0.0370 0.2573
Abs.Std.Dev. 0.0157 0.0025 0.0044 0.0287 0.0005 0.0011
Rel.Std.Dev. 1.78 0.54 0.28 0.05 1.30 0.43

Conclusion Authors
Thanks to the unique properties of the XFlash detector, Dr. Uwe Gerhard Schneider
the quick monitoring of the main element composition of Dr. Heiko Roland Re
limestone including MgO in the daily routine is feasible with Alexander Seyfarth, Dipl. Min.
the benchtop EDXRF spectrometer S2 RANGER. Bruker AXS

High precision is achievable due to the low dead time and

high usable overall count rate of the XFlash detector. The
all-in-one design with system controller and TouchControl
as well as the vacuum pump in the benchtop instrument
allows applications like this to be performed outside of a
clean laboratory.
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All configurations and specifications are subject to Bruker AXS GmbH
change without notice. Order No. DOC-L80-E00082.
2007 Bruker AXS. Printed in Germany. Karlsruhe, Germany
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