Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
APPLICATIONS AND PERSPECTIVES OF A NEW INNOVATIVE
XRF-XRD SPECTROMETER IN INDUSTRIAL PROCESS CONTROL
D. Bonvin, R Yellepeddi
ARL Applied Research Laboratories S.A., 1024 Emblem (Switzerland)
A. Buman
ARC Applied Research Laboratories, Dearborn, MI 48120 (USA)
1.
INTRODUCTION
Wavelength Dispersive X-ray fluorescence (WDXRF) is a well established technique for
process control in various industries. Its versatility in handling both conducting and nonconducting solids, its accuracy and excellent precision for the majority of the elements and
the wide dynamic range (from ppm to 100%) gave WDXRF the place it enjoys in the process
and quality control. Elemental analysis of raw materials, intermediate products (sintered,
calcinated or electrolysis related) and final products (cement, mining, pure metals and alloys)
is routinely carried out using a typical configuration with about 10 to 20 XRF
monochromators for rapid analysis and an XI@ goniometer for flexible analysis of other
elements. In the metals industry, XRF is employed in conjunction with optical emission
techniquesfor a more complete analysis.
Due to the ever increasing demand for the detection and reliable analysis of trace elements in
the production of pure metals as well as for the tighter control of alloy or final product
compositions, there is a need for enhanced sensitivities in XRF and correspondingly lower
limits of detection. In addition, there are needs to monitor specific phases or compounds
either in the raw materials or in the intermediate products for better utilization and process
optimization. Since XRF is essentially capable of measuring total elemental composition
only, wet chemical methods are generally used for the analysis of a given compound, for
example free lime in cement clinkers, differentiation of iron oxides in terms of magnetite and
hematite content, analysis of Fe2+ (FeO) in sinters or alumina related phases etc. These
methods are not only time consuming but are usually off-line with respect to the process
integration. X-ray diffraction can, in suitable cases,quantify the different forms of iron oxides
in ores or the Fe2+in sinters or distinguish alpha-A1203in alumina, or free CaO in clinker, etc.
However, a traditional X-ray diffractometer can hardly be justified for such on-line process
control applications due to its complexity, its poor repeatability and the maintenance costs
involved.
The usefulnessof having both XRF and XRD data on the same sample has been discussed
earlier’. Various combinations using WDX and EDX techniques have been proposed’.The
possibility of an energy dispersive diffraction/spectroscopy was first developed by Giessen
and Gorden and Buras et.a1.2’3The occurrence of diffraction peaks in an energy dispersive
XRF spectrum has been described4.Prediction and detection of diffraction peaks in an energy
dispersive XRF spectrum of a given sample and their exploitation in some applications has
been discussed4.Quantitative phase identification and analysis using the data from XRF and
XRD has been demonstrated in cases such as synthetic corrosion product, limestone and
mullite5. It was hoped that such a combined analysis would become available in a single
program5.A combined XRF and XRD instrument for on-line processcontrol applications was
described earlier 6. This system is based on a diffraction tube excitation of the sample and
126
126
This document was presented at the Denver X-ray
Conference (DXC) on Applications of X-ray Analysis.
Sponsored by the International Centre for Diffraction Data (ICDD).
This document is provided by ICDD in cooperation with
the authors and presenters of the DXC for the express
purpose of educating the scientific community.
All copyrights for the document are retained by ICDD.
Usage is restricted for the purposes of education and
scientific research.
DXC Website
– www.dxcicdd.com
ICDD Website
- www.icdd.com
Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
separate proportional counters to detect diffracted beams and fluorescence radiation. An
integrated XRD-XRF system for the on-stream analysis of slurries was also described earlier’.
Here again, a standard XRD platform is used with fixed geometry goniometer and an EDX
detector for the XRF analysis. A combined XRD and XRF system for portable and remote
applications (planetary explorations) has been developed ‘. Built around low power excitation
and CCD position sensitive detector, such an instrument was shown to be feasible and
applicable
2.
INSTRIJMENTATION
Taking into account these analytical needs, a new X-ray spectrometer has been developed
(Figure 1) which integrates both X-ray fluorescence and X-ray diffraction in one single
instrument (Figure 2).
I‘l&pl:g.~.‘ ( h.Y.S .%?oiotI of 1he itr!egl~rl/ed XIU~AK/ 1 .yec/mniefer
fTiprr 2:
Irl/e.gralior/
nairrtnwnt:
qf Xh!F ami XfW IN /he .sarne
me xample, one it~slrunwr~l, one
L7~lCllj5l.S
The salient features of this new X-Ray instrument are listed below:
.
Modular construction enabling the selection of analytical devices such as XRF
goniometer, XRF monochromators and integrated XRD system. Most appropriate
conligurations can be defined to achieve speed of analysis, sample throughput or limits of
detection as required.
.
High sensitivity thanks to optimized X-ray optical design for monochromators and
goniometers.
.
Latest generation end-window tube with Rh anode providing broad spectrum excitation.
Extra-thin window (75 micrometers) increases sensitivity for light elements. 70 kV excitation
provides higher sensitivity for heavy elements.
.
Geometry with X-ray tube above sample preventing damage to instrument in case of defective
samples (pressed pellets) and ensuring high uptime in routine use.
.
Fast, simple and highly reliable sample introduction system.
.
Fast gearless XRF goniometer with such positioning accuracy that precision is equivalent to
tixed channels. Allows also semi-quantitative and standardless analysis through state-of-theart QuantAS and UniQuant software options.
.
Integrated XRD system providing XRD measurements with the same tube on the same
sample.
.
High stability of analysis thanks to global and local thermal control systems.
.
WinXRF software compatible with Windowsi TM NT environment, integrating analytical
expertise in its Analytical Assistant to help the operator through the use of the spectrometer.
.
Modem support available to prevent or diagnose instrument or analytical problems.
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Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
3.
128
APPLICATIONS
3.1. IRON AND STEEL INDUSTRY
The analytical needs of the modern iron and steel industry (see Figure 3 below) increasingly
demand more comprehensive and process-integrated instrumentation. Two trends seem to
emerge in the way the analytical instruments are positioned in this industry: there is a clear
move towards decentralization of the measurements and there is a need for higher levels of
information content from each analytical instrument. Indeed, most iron and steel
manufacturers would like to see that the analytical capability moves closer to the process
where the answer is truly needed
A
TOTAL IRON X-RAY ANALYZER
mplele an- I&immiy In a d&c hstmment
Iron ores
Hematitqhlagnetite)
Low dKh$
dloy
1
:;,;
.* $
Coating thiekness(nqh2)y
monoelemcnt
on shd
Eli,
plate
Fiqure 3:
Typicul applications in the iron and steel industry for an integrated XRF-XRll
spectrometer
3.1.1 Analysis of hematite and magnetite in iron ores
Figure 3 shows an XRD scan on three iron ore samples. Two distinct peaks can be seen: the
peak around 2.96 Ang. is due to magnetite (Fe303) while the peak around 2.7 Ang. is due to
hematite (Fe,O,). The peak intensities are quite high allowing their use for quantitative
analysis based on peak intensities as there is no observable peak shift as seen in Figure 4.
However, the XRD program allows a search for the exact position of the peak before
measuring the intensity. This is particularly useful if iron ores of different origin are mixed
and slightly varying polymorphic structures exist. It is also possible to do a peak integration
with or without suitable background correction.
40
M
F JI
2 18
.$ II
g *o
1 II
II
8
I
0
1
Bare currr witho”, correctionr
I
I
50
7
I
Fe304-II
-,A+
3.1
,-&&J&.&
3.0
2.9
dspocing
2.8
(Alptrom,
2,
2.6
4
1
Fiqure 4:
XRD scans on 3 iron ore samples showing
the hemafite and magnetite phases
p
$6
r’
-I
JO
j
3”
20
JO
60
80
100
bure 5:
CRD calibration curve of Fe203 in a series
_
ot u-on ore samples
128
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Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
129
Figure 5 presentsthe calibration curve for the hematite phase in a series of iron ore samples.
The accuracy of the XRD measurementreflects that of the wet chemical method. One of the
most important aspects of the integrated XEW system is its reproducibility and long term
stability. The XRD measurementsbenefit from the same optical encoder technology used on
the XRF goniometer as well as from the vacuum environment and the high precision of the
sample positioning system. Apart from the quantification of different mineral species in the
iron ore, the XRF part of the instrument is also used for analysis of trace elements or oxides
presentin the sample.
3.1.2 Analysis of Fe0 in sinters:
Analysis of Fe0 in sinters can be made much faster and on-line with the help of the integrated
XRD system,typically in less than 100s with very good precision. A series of sinter samples
were measured to establish the calibration curve using concentrations determined by wet
chemistry.
A typical range of Fe0 may be between 4 to 9%. This means that very high sensitivities are
necessaryto achieve good precision. Thanks to the closely coupled optics, the integrated
XRD system offers the necessary peak to background intensities to achieve satisfactory
performance.
Figure 6 shows a calibration curve obtained for a series of sinter samples. Excellent
correlation is obtained between the XRD intensities and the chemical concentrations of FeO.
Table 1 provides the corresponding regression results. A typical standard error of estimate
(accuracy) of around 0.2% is achieved.
8h
4.2
3.8
4.0
%
I
3.6
3.4
P
3.2
2
if
Sinter
Base Curve wihtoutCar,ectionr
4.4
2.6
3.5
4.0
4.5
5.0
5.5
Fe0 Concentration
6.0
6.5
P/o>
Figure 6: XRD calibration for Fe0 in sinters
7.0
T
Inten--Concentration of
PC sity
Nr.
Calcul.
Nominal
Kcps
1
3.5583
5.41
5.0
2
3.5384
5.3
5.38
4.4
4.27
3
2.9626
4
3.5743
5.4
5.44
5
4.8
4.79
3.2299
5.6
5.78
6
3.7489
7
5.49
5.5
3.5981
3.4294
5.2
5.17
8
6.4
6.09
9
3.9115
6.2
5.93
10
3.8248
5.6
5.77
11
3.7422
5.74
5.8
3.7274
12
4.6
4.51
13
3.0838
0.20
Standar Error of Estimate:
l-
Difference
Absolute
0.41
0.08
-0.13
0.04
-0.01
0.18
-0.01
-0.03
-0.3 1
-0.27
0.17
-0.06
-0.09
Table I: XRLI calibration results of Fe0 in sinters
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130
Table 2 shows short term repeatability results on a sinter sample. Since the instrument is
capable of analysing all the elements or oxides by XRF together with the Fe0 concentration
by XRD in the same sample, one can effectively combine the results from the two methods
and exploit the synergy between total elemental concentration and the specific phase content
of the same element. The standard deviation shown in Table 2 for most of the constituents
doesconfirm the suitability of the instrument in a typical processcontrol environment.
Run
Fe0
I>
2>
3>
4>
5>
6>
7>
8>
9>
lO>
ll>
A%
Sd
Sd%
Table2.
-*
SiOz
8.32
8.31
8.30
8.32
8.30
8.32
8.30
8.30
8.29
8.31
8.32
Fe
Total
56.25
56.24
56.25
56.25
56.26
56.27
56.27
56.27
56.27
56.27
56.28
5.81
5.82
5.81
5.82
5.83
5.82
5.82
5.83
5.82
5.83
5.82
8.31
0.01
0.13
56.26
0.01
0.02
5.82
0.01
0.10
CaO
Ml@
TiOz
Mn
S
P
V
2.14
2.13
2.13
2.14
2.14
2.13
2.13
2.13
2.14
2.14
2.14
10.21
10.21
10.20
10.21
10.20
10.21
10.20
10.20
10.21
10.20
10.20
1.78
1.79
1.79
1.79
1.79
1.79
1.79
1.79
1.78
1.79
1.79
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.32
0.32
0.32
0.32
0.32
0.32
0.32
0.32
0.32
0.32
0.32
0.004
0.004
0.004
0.004
0.004
0.004
0.004
0.004
0.004
0.004
0.004
0.098
0.098
0.098
0.097
0,099
0.097
0.098
0.099
0,099
0.097
0.099
0.029
0.028
0.029
0.029
0.030
0.029
0.030
0.028
0.030
0.029
0.030
2.14
0.00
0.23
10.20
0.00
0.04
1.79
0.00
0.17
0.22
0.00
0.39
0.32
0.00
0.39
0.004
0.000
1.748
0.098
0.001
2.130
2.43
0.00
0.11
A1203
Short term repeatability results on sinter sample using the integrated XRD-XRF spectrometer
3.1.3 Direct Reduced Iron:
Direct Reduction (DR) has been defined as the processof reduction of iron oxides to metallic
iron using a lower temperature than required for a conversion to liquid state. The iron oxides
can be in the form of sized ores, concentrates,pellets or mill scale etc. The reduction process
itself can be gas based or coal based.Direct Reduced Iron (DRI) is a metallic product which
is used as a feedstock for electric arc furnace steelmaking, in blast fwnaces, and in other iron
and steelmaking applications. Its main advantagesare a low level of impurities and chemical
and physical consistency.Hot Briquetted Iron (EIBI) is a densified form of DRI.
The DRI process is being implemented in various parts of the world thanks to its many
advantages.Since the process involves reducing the iron ore directly using a gas mixture of
carbon monoxide and hydrogen, for example, the analysis of iron ore as it goes through a
seriesof reactors would allow a continuous control of the reduction process.It is obvious that
the concentration of iron oxide (hematite for example) decreasesto near zero levels when the
most of the iron is in the metallic form. The integrated XRF-XRD spectrometer,named in this
case Total Iron X-ray Analyzer may be used to monitor this processby measuring the oxide
content by XRD, total Fe content by XRF and the difference accounting for the metallic Fe.
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131
3.2. ALUMINIUMINDUSTRY
Production of aluminium involves electrolysis of aluminium oxide. Starting from the raw
materials (bauxite, aluminium bearing minerals) through alumina to aluminium metal and its
alloys, XRF can be positioned in different areasof processand quality control in this industry
(see Figure 7 below). X-ray diffraction (XRD), on the other hand, is commonly used, for
example, to perform the electrolytic bath analysis in addition to any other off-line
applications.
luEAL
ALUMINIUM
X-RAY ANALYZER
Acompleteanntysislaboratoryiuasingle~
Alumlns
(a-Al203)
Electrolyte Bath
;cess AlF3,C&?, BR:
Alumtntum metal
Alloys
,Fisure 7:
Typical applications in the aluminium industry for an integrated XRF-Xm spectrometer
Figures 8 and 9 show as examples the calibration curves for the excessAlF3 and total calcium
respectively, using the integrated XRD system of the Total Aluminium X-Ray Analyzer.
Figure 10 shows the calibration curve obtained for a-Al203 in a series of alumina samples
using the sameXRD system.
MVR Graphical
Results:
XRD for excess AIF
/
sase curve WIthoUt CorreCtlo”B
23.6
23.2
t 228
22.4
$D 22
21.6
E
f
B
21.2
0
2
4
s
Cancmtratlan [%,
8
i-:r:-:’
4.8
4.9 6
5.1 6.2
Concentration ml
:
I
1
Figure 8: XRD calibration curvefor the excessof AlF3 in Figure 9: XRF calibration curve for the total calcium
a series of bath samples
in the bath samples
II
MVR Graph14
XRD of Alpha4203
Results:
in Alumina
Base Curve without Corrections
Figure IO: XRD calibration curve for the a-AlJO in a
series of alumina samples
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132
3.3 CEMENT INDUSTRY
The analytical requirements of the cement industry have evolved in the past few years to
encompass a wide range of materials and qualities. While it is difficult to substitute the
different physical and chemical methods used in a cement laboratory by a single technique,
most cement manufacturers are looking for rationalization and integration of analytical
methods. This is in accordancewith the drive to (a) optimize the use of raw materials and
additives, (b) reduce the production costs, (c) improve and stabilize the quality and (d) keep
the maintenance and running costs under control. In addition, environmental issues are
becoming more and more important in the cement industry both in terms of using the kiln to
incinerate and eliminate waste products and using “by-products” from other industries as
fillers, i.e. coal ash, metallurgical slags, silica dust etc.
TOTAL CEMENT ANALYZER
A~pMecementat+slshbora~inazin~madtb~e
(Slags, Fly Ash,
Limestone, etc.)
Cement
(Heavy mctsl, In du.st)
Fiaure 11:
Typical applications in the cementindustryfor
an integrated XRF-Xm spectrometer
While the role of XRF in the analysis of major and
minor oxides in the raw materials, clinker, cement
and additives is universally accepted, the use of
XRD for the analysis of free lime in clinkers and
other crystalline phases such as limestone in the
process of precalcination or as an additive in
cement has been limited until recently. Only an
integrated XRD system can be justified in such online process control applications due to its
simplicity of use, high repeatability and the low
maintenance costs involved. A summary of various
applications in the cement industry is given in
Figure 11 and in Table 3.
TOTAL CEMENT ANALYZER
XRF
Fixed channels
l
l
l
Simultaneous and
rapid analysis
(<4Os) CaO, SiO,,
AJO,, Fe203,
MgO, SO,, etc.
Higher throughput
Dedicated
programs
XRD
System
Goniometer
l
l
l
l
Sequential and flexible analysis
Analysis time (analysis of major & minor
oxides) (~2 min)
Analysis of sulfide versus sulfate in slags
(as additive in cement)
Semi-quantitative programs QuantAS and
Uni-Quant for standardless analysis of
samples from :
quarry, coal ash, additives (like fly ash:
alumino-silicates, pozzolans, slags, by-pass
(Na, Cl, S ...) gypsum (minors & traces),
heaw metals on electro-filter dust. etc.
l
l
l
l
l
l
Free Lime in clinkers
Limestone additions in
cement
Pozzolan additions
Clinker phases (C,S,
C,S, C,A and C,AF)
Hot meal (CaO vs
CaCO,)
Gypsum phases, etc.
Table 3: Summaryof typical applications using the ARL ‘s Total CementAnalyzer
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133
3.4. STANDARD-LESS ANAL YSIS
From the analyst point of view, one of the most useful recent developments in WDXRF has
been the availability of semi-quantitative or so called “standard-less” analysis programs.
These programs enable to handle all kinds of samples irrespective of the availability of
matching standardsand calibrations. A universal goniometer covering most of the elements
from Boron to Uranium is used for this purpose.
The semi-quantitative analysis can be based on a global scan followed by spectral processing
(QuantAS) or peak and background measurementsat fixed spectral positions followed by
intensity processing(UniQuant@).The accuracy and reliability of these programs is improving
constantly as more efticient matrix correction algorithms, overlap and background correction
models are developed. Applications such as alloy sorting or characterization of specialty
alloys, on-the-spot analysis of raw materials, analysis of irregular solids etc. can be handled
using these programs. Indeed, both QuantAS and UniQuant@ programs bring a very high
value to the XRF goniometer by fully exploiting its flexibility, precise angular positioning and
optimized collimator-crystal-detector combinations.
Although the X-ray instruments in any industrial process control are predominantly applied
for the analysis of routine samples, there is still a need for flexibility to handle ad hoc or
occasional samples.For example, the quality of the incoming raw materials or fluxes or coal
or environmental dust or any other specialty products may need to be characterizedfrom time
to time. Difficulty arises when these non-routine samples do not fit into any of the calibrated
programs. Semi-quantitative programs can handle such situations and report the
concentrationsdirectly. The following three examples (tables 4, 5 and 6) illustrate the typical
performance of such programs in comparison with certified concentrations
---IZn
_--.
Al
>
1
I
25.3%
5.10%
25.2%
5.18%
~~~
I
Cl
Al
Ca
S
I
650o~m
530ppm
1
/
I
740ppm
650o~m
540ppm
/
I
I
1Oppm
I
31 wm
1
Table 4: Sample BERM CDA 863 - Copper Alloy
Table 5: Sample NlsT 195 - Ferro-Silicon ---------->
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Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
Concentrations
Element
I
Fe
Given
1
UQ
/
31.2%
2.38%
Mn
1
I
30.5%
1
0.941%
2.20%
0.910%
1
0.928%
Ta
-.
Si
Al
0.752%
0.807%
0.790%
0.382%
0.198%
0.414%-
0.134%
0.164%
0.240%
La
265ppm
102ppm
280ppm
Ti
232ppm_.---_---
292 ppm
270ppm
202 ppm
180ppri____-170
--___ppm
v
Cl
I
2.82%
2.83%
1
30.8%
j QuantAS
Table 6: Sample BS 162 - Maraging Steel
4.
LINKING THE INSTRUMENT
AUTOMATION
TO THE PROCESS THROUGH
There exists in process control industries requirements for simple automation requirements
where samples are available only in one single form, typically pressedpellets in steel rings or
cylindrical metallic samplesof identical size. In these casesa large sample changerpositioned
directly in front of the instrument can be linked to a transport belt which brings the prepared
samplesfrom the automatic preparation machines to the instrument. The griper of the sample
changer can move on both X and Y axis in order to position itself precisely at desired
positions above the surface of the magazine. The griper picks up the sample from the belt and
brings it to the loading port of the instrument to be introduced into the vacuum chamber of
the spectrometer.
The sample identification and the analytical program selection can be done through software
connection from a remote PC using the standardanalytical software. Alternatively an external
computer system can act as master of the whole automation system. Automation of analysis
can be performed not only for production samples but also for control standards,setting-up
samples and type standards. After the analysis the sample can be returned to the same
transport belt or to a secondtransport belt (Figure 12) or filed in three classification baskets
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Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
Belt from the right
of instrument
Belt from the rear and
left of instrument
transport
belts
Belt from the left of
instrument
L
&we
12: Illustration
qf the various possibilities to link rrausport hrlt.r to the X-Y sumpIt changer.
When full automatic operation is required, the instrument can be connected to automatic
preparation machines through a robotic sample manipulation system (Figure 13). This flexible
tool for automation works as the brain and arm of the whole analysis process. Thanks to the
use of an industrial robot for all manipulation operations,
it can handle multiple sample
forms. It manages the sample introduction, registration, preparation and analysis, as well as
the priorities between analysis of production samples, measurement of control standards,
running of setting-up samples, type standards or manual samples. Sample sorting, marking or
filing are performed quickly and efficiently. The automatic sample manipulation system
works in order to minimize sample turnaround time. Instrument control through on-line
Statistical Process Control (SPC) and standardization are tasks which are integrated in the
normal routine work of the automation system. They are only performed when required and at
times when analy: <is C
to /he loadit~g port of
I~?~wrr 13: The roboil
the .spectrometer
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Copyright(C)JCPDS-International Centre for Diffraction Data 2000, Advances in X-ray Analysis, Vol.42
5.
CONCLUSIONS
In conclusion, the ARL 9800 X-ray spectrometeroffers the state-of-the-art instrumentation to
meet the present and the future analytical requirements of process control industries, in
particular in the iron and steel, aluminium and cement industries. The modularity, reliability,
reproducibility and the ease of use through total integration are the key features of this new
instrument. The integration of the well establishedXRF technique in conjunction with XRD
is realized in a single instrument with a view to facilitate the most comprehensiveanalysis of
raw materials and products. The instrument can be configured and optimized with various
analytical modules to handle fast routine elemental analysis as well as analysis of non-routine
samples, The compact size of this new instrument is compatible with its integration into
simple or state-of-the-art automated systems linking it to automatic sample preparation
equipment.
6.
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