QUALITY AND CERTIFICATION
X-RAY SPECTROSCOPIC METHOD FOR CHEMICAL ANALYSIS
OF PERICLASE POWDERS
L. V. Mironova,
E. V. Murashko,
and L. V. Mikhailova
Translated from Novye Ogneupory, No. 2, pp. 51 – 53, February, 2004.
An x-ray fluorescence spectroscopic analysis in the incoming inspection of raw materials for the production of
periclase powders is developed. Optimum conditions for sample preparation are described and a metrological
characterization of certified mixtures is given. The advantages of the newly-developed method, based on the
use of a Spectroscan-V x-ray spectrometer, are emphasized.
In the production of high-temperature refractories, raw
material control is an issue of special concern because of its
direct relevance to the processing technology, competitive-
ness of the final product, and rejection of defective articles
whose quality fails to meet normative requirements.
In 1999, at the Magnitogorsk Iron and Steel Works a
shop for production of periclase-carbon materials for the re-
fractory lining of steel ladles was put into service. The pre-
cursor materials in the refractory production were sintered or
fused periclase powders, carbon-containing additives, and a
composite binder. Simultaneously, an incoming inspection of
all purchased materials was organized. Special attention was
given to the quality of periclase powders.
Standard methods for determining the chemical compo
sition of periclase have been developed . However, these
methods are time-consuming, laborious, and uneconomical
and, most importantly, they fail to meet the technologist’s re
quirement for prompt operational information on the quality
of materials used. To remedy the situation, a decision was
made to use x-ray fluorescence analysis. An analytical unit
composed of a Spectroscan-V x-ray spectrometer and auxil
iaries for sample preparation was purchased from the
Spectron Research and Production Association (St. Peters
burg, Russia). The instrument in question was a portable
scanning crystal x-ray spectrometer.
The x-ray spectrometer was designed using an advanced
technology for instruments of this class. Combining a high-
transmission x-ray optical scheme and a BKhV-17 sharp-fo
cused x-ray tube made it possible to design a desktop spec-
trometer with superior analytical parameters. The inner com-
partment could be evacuated, which made it possible to ana-
lyze light elements from Ca
. The test specimen was
accommodated outside the vacuum, that is, materials in any
aggregate state could be investigated. The instrument re-
quired no tap-water cooling for the x-ray tube, and no ar-
gon-methane mixture from a cylinder was needed for the gas
flow proportional detector. Alternatively, a closed-loop cool
ing system for the x-ray tube and a sealed-off proportional
x-ray detector with a xenon filler were used.
A set of measures was considered to provide for the
on-line quality control of precursor periclase powders. The
main program installation was checked and put in operation.
Calibration of the instrument was carried out and positional
calibration was effected to match the goniometric scale with
tabular wavelengths of the elements. For each crystal the ca
libration was carried out in the automatic regime with refe
rence to a specified set of analytical lines.
Optimum conditions were provided for preparation of
the periclase powder samples for analysis. Because of the
high abrasive ability of periclase, the mill-ground samples
became contaminated with elements of the milling equip
ment material (Si, Fe). These elements are also impurities to
the precursor periclase powder; therefore, to maintain these
elements within required specifications, a grinding techno
logy was developed to provide the needed fineness of grind
ing and prevent the analyzed material from contamination.
A laboratory sample  of periclase powder was drawn
and ground using different techniques. The grinding equip
Refractories and Industrial Ceramics Vol. 45, No. 3, 2004
1083-4877/04/4503-0222 © 2004 Plenum Publishing Corporation
Magnitogorsk Iron and Steel Works (MISW) Joint-Stock Co.,