ISSN 00201685, Inorganic Materials, 2015, Vol. 51, No. 14, pp. 1438–1441. © Pleiades Publishing, Ltd., 2015.

Original Russian Text © V.A. Simakov, V.E. Isaev, 2014, published in Zavodskaya Laboratoriya. Diagnostika Materialov, 2014, Vol. 80, No. 12, pp. 16–19.

ANALYSIS OF SUBSTANCES

XRay Fluorescence Determination of Magnetite Iron

in Iron Ores after Preliminary Magnetic Separation
V. A. Simakov and V. E. Isaev
Fedorovsky AllRussia Research Institute of Mineral Resources, Moscow, Russia
email: simvlad44@mail.ru
Received September 1, 2014

Abstract—The technique for determining the magnetite iron content in iron ores by Xray fluorescence after
preliminary extraction of magnetic fraction by using a magnetic separator is proposed. Separation of the mag
netic and nonmagnetic fractions occurs with sufficient completeness and accuracy at a particle size in the
sample in the range of –0.074 to +0.044 mm. At smaller grain size, the quality of separation sharply worsens.
Mixing of a weighed sample with nonmagnetic powder before separation provides satisfactory accuracy of
recovery of the magnetic fraction even in the case of a very finely powdered sample. Application of an Xray
fluorescence energy dispersion spectrometer makes it possible to perform a qualitative assessment of separa
tion by comparison of spectra of scattered and fluorescent radiation after each separation cycle.

Keywords: magnetite iron, magnetic separation, Xray fluorescence analysis, iron ores
DOI: 10.1134/S0020168515140101

Magnetite ores are the main industrial type of iron
ores. To assess the ore quality, information about the
magnetite iron content (MIC) should be available
when controlling and adjusting the process of ore
treatment. The existing physical methods of MIC
determination from the values of magnetization or
magnetic susceptibility are of high performance, but
the correct results require calibration of instruments
on the basis of reference specimens which should have
known MIC value and be comparable to the studied
specimen in terms of composition and magnetic prop
erties. This latter condition cannot always be guaran
teed when searching for and exploring deposits. The
universal method of MIC determination is magne
tochemical [1]. However, in some cases, in manual
extraction of the magnetic fraction using a constant
magnet according to the technique [1], the reproduc
ibility is unsatisfactory. In addition, the analyst cannot
control the completeness of separation between the
magnetic and nonmagnetic fractions in a sample.
The present work attempts to overcome these diffi
culties by way of using (a) a magnetic separator with an
alternating magnetic field for separating the fractions
and (b) Xray fluorescence analysis for controlling the
separation completeness and determining the iron
content in the initial sample and magnetic fraction.
The iron content was determined on an ERA
energy dispersion spectrometer equipped with a Si(Li)
detector (resolution of 150 eV on the MnKα1 line). A
BS6 Xray tube with molybdenum anode (U = 40 kV,
I = 40 μA) was the source of the initial Xray spectrum.
The FeKα1 line was used as the analytical one. The
examined specimens were powdered samples with a
grain size of less than 70 μm. Each sample was irradi
ated from below. Powdered samples were closely
packed in a cuvette with the bottom being permeable
to the studied spectrum of Xray radiation. Matrix
effects were taken into account by means of a compar
ison line—incoherently scattered radiation [2]
MoKα1 of the anode of the Xray tube. At a constant
factor of incoherent scattering MoKα1 and in the
absence of surges of absorption of elements of a sample
between the compared lines, this ratio does not
depend on the total composition of a sample, but
depends only on the content of the determined ele
ment. The influence of sample composition in the
presence of selective effects was taken into account
with the help of semiempirical influence coefficients
[3] which were found by using samples with known
iron content and noticeable amounts of interfering
elements.
The content of a determined element was calcu
lated by the expression [3]
I 1
C i = i 
, (1)
I nc A i +
∑B ij I j
j
where
I i = N i – a i I nc – b i – ∑dk
ik I k . (2)
Ni is the set of pulses at the analytical line; Ii is the
intensity of the analytical line; Inc is the intensity of
incoherently scattered radiation of the anode line;

1438
 XRAY FLUORESCENCE DETERMINATION OF MAGNETITE IRON 1439

Table 1. Results of determination of magnetite iron content in SCS in the content interval of 10.0–29.9 wt %
Iron content, wt %
GSO or OSO name
C1 (by specification) C2 (determined) C1/C2
519–84Π 10.65 1.54 0.9865
2270–82 18.89 2.27 1.0109
3032–84 20.2 1.64 0.9983
3026–84 14.38 7.88 1.0000
3027–84 15.6 1.20 1.0185
3028–84 16.74 6.02 1.0000
3030–84 13.84 3.33 0.9862
OSO 260–92 18.03 4.99 1.0026
2742–83 25.9 4.84 0.9911
dr = –0.065 (n = 9); tcalc = 0.19 < ttabl = 2.26—the systematic error is statistically insignificant; Sr = 1.0; σper (10.0–19.9 wt %) = 1.6;
σper (20.0–29.9 wt %) = 1.0.

Table 2. Results of determination of magnetite iron content in SCS in the content interval of 30.0–69.0 wt %
Iron content, wt %
GSO or OSO name
C1 (by specification) C2 (determined) C1/C2
2743–83 37.02 36.99 1.0008
1480–84Π 33.14 33.13 1.0000
1865–80 38.2 38.13 1.0018
OSO 182–89 38.63 38.73 0.9974
5405–90 54.83 55.06 0.9958
2744–83 52.84 52.27 1.0108
6678–93 68.26 69.0 0.9890
OSO 181–89 63.18 63.08 1.0016
457–74 56.0 56.11 0.9981
1195–79 56.21 55.75 1.0082
281–86 43.2 43.37 0.9960
(457–74) + (281–86) (1 : 1) 49.6 50.09 0.9903
dr = –0.065 (n = 12); tcalc = 0.42 < ttabl = 2.18—the systematic error is statistically insignificant; Sr = 0.7; σper(30.0–39.99 wt %) = 0.8;
σper(40.0–69.0 wt %) = 0.7.

dik is the overlapping factor (contribution of intensity
from the Ik line to an increase owing to overlap of ana
lytical line intensity); ai and bi are the coefficients of
linear dependence [4] of background intensity at the
analytical line on intensity of incoherently scattered
radiation of the characteristic anode line (MoKα1) of
the Xray tube; and Ai and Bij are the influence coeffi
cients. In the absence of selective effects and at a con
stant coefficient of incoherent scattering, Bij = 0 and
st –1
Ai = [ C i ( I nc /I i ) st ] , where the uppercase index “st”
refers to the compared specimen. Bij considers both
the selective absorption of radiation from the com
pared line by element j in a sample and the change in
the coefficient of incoherent scattering of radiation
from the compared line owing to the effect of this ele
ment. The effects of additional excitation when deter
mining the iron content in iron ores can be neglected.
Tables 1 and 2 present the results of iron content
determination in standard composition specimens
(SCS) of rocks and ores in the interval of iron content
from 10 to 69%. Here, the interfering influence of iron
was taken into account when computing the contents
by expression (1).
The metrological characteristics of the technique
were assessed in accord with the standard [5]: the rel
ative systematic error (dr), standard deviation (Sr), and
permissible error for different content intervals (σper)
were calculated. As is seen from Tables 1 and 2, the
accuracy of Xray fluorescence analysis satisfies the

INORGANIC MATERIALS Vol. 51 No. 14 2015