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Development of X-Ray Fluorescence Analysis in Russia in 1991-2010

Article in Journal of Analytical Chemistry · November 2011

DOI: 10.1134/S1061934811110116

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ISSN 10619348, Journal of Analytical Chemistry, 2011, Vol. 66, No. 11, pp. 1059–1072. © Pleiades Publishing, Ltd., 2011.
Original Russian Text © A.G. Revenko, 2011, published in Zhurnal Analiticheskoi Khimii, 2011, Vol. 66, No. 11, pp. 1174–1187.

REWIEVS

Development of XRay Fluorescence Analysis

in Russia in 1991–2010
A. G. Revenko
Institute of the Earth’s Crust, Siberian Branch, Russian Academy of Sciences, ul. Lermontova 128, Irkutsk, 664033 Russia
Received January 21, 2010; in final form, April 30, 2011

Abstract—A survey attempted to examine the results of studies in Xray fluorescence (XRF) analysis per
formed by Russian authors for the period from 1991 to the present time is given. This proved to be quite a chal
lenge, since the number of articles published only on the theory and practice of XRF (excluding the develop
ment of equipment) exceeded 500. Therefore, the author had to limit himself to a more detailed presentation
of only several important achievements. Further information, if necessary, can be found in the cited reviews.

Keywords: Xray fluorescence analysis

DOI: 10.1134/S1061934811110116

A number of reviews have been published for the
considered period [1–26]. The stateoftheart of
energy dispersive XRF at the beginning of the 1990s
was reviewed by Revenko [1], while at the beginning of
the 21st century, in the works by Yakubovich and
Ostroumov [8], Pshenichnyi et al. [16], and Serebrya
kov [22]. The use of total external reflection Xray flu
orescence (TXRF) spectrometers was discussed by
Losev et al. [2], Revenko [24, 26], and Alov [25]. The
stateoftheart and development trends, as well as the
use of XRF with excitation by synchrotron radiation
and microfluorescence using capillary optics, are pre
sented in the reviews of Kumakhov, Dabagov, and
Revenko [7, 9–14, 20, 21, 23]. Different representa
tions of the constraint equations in XRF are discussed
in [4]. A number of reviews are devoted to the prob
lems of the use of the method for determining the
composition of individual samples: geological and
environmental [3, 12, 13, 26], organic materials [5],
and samples containing platinum group metals [17]
and for the determination of trace substances in vari
ous materials [6]. The applications of XRF in the agro
chemical service (analysis of plants, animal feed, soil,
and other samples) are summarized in the review by
Pukhovskii [15].
A number of publications considered the historical
aspects of XRF. The publication by Ostroumov et al.
[27] was devoted to the laboratory services of the All
Russian Institute of Mineral Resources. In this insti
tute, the theory of the interaction of Xray radiation
with matter was developed already in the 1940s and
1950s, and equipment was created to disperse the radi
ation into a spectrum for recording (M.A. Blokhin,
I.V. Sorokin). In the 1950s, the method began to be
widely used for the analysis of mineral raw materials
and their products. New ways were developed to con
sider the effect of the chemical composition of sam
ples on the intensity of analytical lines, for example,
the standardbackground method, the substrate
method (I.V. Sorokin, V.P. Bykov, etc.). A methodol
ogy and software to calculate the concentration of ele
ments in the multicomponent analysis of rocks and
ores were created (V.I. Sorokin, V.A. Simakov,
S.V. Kordyukov) using a multichannel spectrometer
(the works of the last period are partially discussed in
this review). Interesting data on the first decades of the
development of XRF in the Soviet Union are pre
sented in the review of Il’in [18]. The contribution of
M.A. Blokhin (1908–1995) to the arrangement of
works on XRF in our country is covered in the article
of Filippov [28]. Centenary of his birth is devoted the
VI AllRussian Conference on XRay Spectral Analy
sis (2008). The career of V.P. Afonin was considered in
one of the reports on this conference [29]. In the third
chapter of the manual [30], the information about the
development of XRF is given and the photos of the sci
entists are presented, who contributed to the develop
ment of the theory and practice of XRay Analysis.
Scientists from Irkutsk did much in solving the prob
lems of XRF. For many years, the Irkutsk State Uni
versity prepared physicists, the researchers in the field
of Xray structural and spectral analysis; its graduates
are currently employed in many laboratories, where
physical methods of investigation are used. Petrov et
al. [31] outlined the history of the establishment of the
analytical laboratories of the A.P. Vinogradov Institute
of Geochemistry (by the way, there is an inaccuracy
in this work: V.P. Afonin supervised the Laboratory of
XRay Spectral Analysis of the Institute of Geochem
istry since 1972, not 1967). Smagunova and Pavlinskii
presented the history of establishment and achieve
ments of the Irkutsk scientific school [32]. Interesting

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1060 REVENKO
episodes, describing the atmosphere of this period,
can be found in the collective work prepared for the
75th anniversary of N.F. Losev [33]. In 2008–2009, an
issue of the journal XRay Spectrometry—Russian–
Mongolian special issue of XRS (2010, no. 1)—was
released at the suggestion of the editorial board of this
journal. In the introduction to this issue [34], the edi
torial board attempted to justify this choice. In fact,
the material is the addition to issues [31–33].
A large amount of information on various aspects
of XRF is contained in monographs [35–44] and text
books [30, 45–48], published in these years. The
monographs of Afonin, Komyakov, Nikolaev, and
Plotnikov [35], Revenko [38], and Borkhodoev [39]
concern general issues. Unfortunately, published in
the 1990s, these books cannot give a contemporary
view of the potential of the method. The monographs
of Borkhodoev and Pavlinskii are reviewed in the jour
nal XRay Spectrometry [49–50]. Pshenichnyi et al.
[36] and Verigin [42] considered the problem of energy
dispersive Xray analysis. In the book of Pukhovskii
[41], there is a section that discussed the features of
specific procedures for studying soil by XRF. Several
papers are devoted to Xray optics [37, 40, 47]. Publi
cation [51] is a bibliography on Xray spectral analysis
and Xray and electron spectroscopy. There are the
following sections (the numbers of books in this sec
tion is indicated in parentheses): general issues, his
tory, and popular literature (9); Xray physics (50); the
effect of chemical bonds on the Xray spectra (14);
handbooks (28); Xray techniques and dosimetry (22);
Xray analysis (89); electron probe microanalysis and
microscopy (47); Auger and photoelectron spectros
copy (18).
Development of the theoretical foundations of the
method. The main results, obtained by Russian col
leagues, are adequately presented in the monograph of
Pavlinskii [43]; the monograph is translated into
English [44]. Several papers have been devoted to
assessing the spectral distribution of the radiation
intensity of Xray tubes of various types. For example,
Finkel’shtein and Pavlova introduced amendments to
the intensity of bremsstrahlung in the longwavelength
region for its absorption at the outlet of the anode and
the contribution of fluorescence excited by this radia
tion [52, 53]. Pavlinskii and Portnoi reviewed the fea
tures of the spectral distribution of the radiation inten
sity of Xray tubes with a grounded cathode [54, 55].
Kitov presented the results of the calculation of the
shape of the spectral distribution of bremsstrahlung
before and after scattering on Alpolarizers of various
thicknesses [56, 57]. Kitov and Moukhachev studied
theoretically the shape of the spectral distribution of
the emission of pulsed throughtarget Xray tubes
[58]. It was noted that increasing thickness of the tube
target leads to an increase in the degree of monochro
maticity of the radiation. The comparison of the spec
tral distributions of bremsstrahlung of the tubes oper
ating at a constant voltage and in a pulsed mode
JOURNAL OF ANALYTICAL CHEMISTRY
showed that with a general decrease in the intensity of
the radiation, the longwavelength component
remained practically unchanged.
Finkel’shtein et al. [59] proposed the ratios for cal
culating the fluorescence intensity and the scattered
primary radiation at the XRF of pulp and pulplike
materials. The ratios are obtained for the model of
pulp, in which the distribution of solid particles obeys
the Poisson distribution. The authors compared the
results of the calculations with the experimental data;
a satisfactory agreement was observed for materials
with the particle size of 500 μm. In subsequent studies
[60–64], the authors have extended this approach to
powders.
Pavlinskii et al. [65–70] calculated the contribu
tion of photoelectrons and Auger electrons, arising in
the test material, into the Xray fluorescence of the
elements with atomic numbers from Z = 5 (boron) to
Z = 9 (fluorine). The calculations were performed for
the case of the monochromatic primary radiation and
for the inhomogeneous radiation of Xray tubes.
The calculations indicated the dominant role of the
photoelectrons and Auger electrons in the excitation
of Xray fluorescence of elements with low Z. This
explains the high fluorescence intensity of these ele
ments under conditions of a low probability of photo
ionization by a relatively shortwave primary radiation
from Xray tubes. The conditions of excitation (the
anode material, voltage on an Xray tube, and the
thickness of the Bewindow), under which the inten
sity of the Xray fluorescence of elements with low Z
would be maximal, are considered. The approach to
the selection of those conditions significantly differs
from that practiced in the XRF of elements with high
Z, and the result is strongly dependent on the chemical
composition of the test material. The resulting expres
sions for the intensity of Xray fluorescence, arising
under the effect of photoelectrons and Auger elec
trons, form the basis for solving analytical problems by
using the prospective method of fundamental parame
ters in the case when elements with low Z are pre
sented in a sample. The contribution of the selective
excitation into the fluorescence intensity of carbon,
nitrogen, oxygen, and fluorine by using Xray tubes
with different anodes and the thickness values of the
Bewindow of 75 to 300 μm was evaluated [70, 71].
The calculations were made taking into account the
contribution of Auger electrons and photoelectrons. It
was found that the contribution of this effect was in
some cases quite substantial.
Borkhodoev evaluated the effect of mass attenua
tion coefficients on the accuracy of the calculation of
the intensity of Xray fluorescence of petrogenic ele
ments [72]. These estimates were made considering
new data on the mass extinction coefficient, published
after 1970. His findings largely confirmed the conclu
sions drawn earlier in [38, 73, 74]. Finkel’stein and
Gunich [75] compared several versions of the extinc
tion coefficients used in the XRF. Finkel’stein and
Vol. 66 No. 11 2011
 DEVELOPMENT OF XRAY FLUORESCENCE ANALYSIS
Farkov attempted to approximate the attenuation
coefficients of Xray radiation in the energy range of
0.1–100 keV [76]. Marenkov investigated the possible
functional representations of the energy dependence
of integral cross sections for incoherent scattering of
Xrays and γrays [77].
The practical approximation of the Sherman for
mula for the fluorescence intensity was suggested by
Pavlinskii and Vladimirova [78]. The new model pro
vided a good agreement between the experimental and
theoretical values of intensity when was verified for
highalloy steels. The authors discussed the possibility
of using the intensities, not corrected by the value of
Xray background, for this new model.
Volkov et al. [79, 80] performed a theoretical
assessment of the detection limits of elements in the
range of 69 < Z < 92 by the Kseries of Xray spectra
with the use of electron accelerators (electron energy
of 1.5 MeV) for the excitation of fluorescence. It was
assumed in the calculations that the bremsstrahlung
target of the accelerator is made of aluminum, which
provides a higher, compared with a target of tungsten,
bremsstrahlung intensity in the range of photon energy
<1 MeV for the electron energies <2 MeV. It was found
that in the case when the electron energy increased
from 1 to 5 MeV, the detection limit for 92U decreased
by 3 times. With increasing Z from 69 to 92, the detec
tion limit became approximately twice higher (worse).
These data show that the implementation of the
experimental setup for the excitation of elements with
such atomic numbers enables the determination of
their concentration at the level of 10–8–10–9% without
complicated sample preparation (chemical precon
centration). Perhaps, such a result was obtained due to
an incomplete accounting of the components of Xray
background. The contribution of the additional exci
tation by scattered radiation in XRF of ionimplanted
layers was estimated by Naumtsev and Volkov [81].
In a series of papers [82–86], Oskolok and Monog
arova investigated the variations of the concept of the
effective wavelength of the primary spectrum of an X
ray tube in the XRF analysis of homogeneous multi
component samples. It should be noted that some pro
fessionals involved in this problem previously, came to
the conclusion that this trend currently has a limited
application in the development of theoretical founda
tions of XRF.
Evaluation of mutual influences of elements. The
theoretical modeling of the mutual influence of the
elements and the evaluation of errors, arising due to
changes in the chemical composition of samples using
the theoretical intensity of Xray fluorescence, are
widely used in the development of XRF procedures.
The stateoftheart of the theory of excitation of flu
orescent radiation enables the accounting of all the
variety of matrix effects: the contribution of the selec
tive excitation of atoms of the analyte element, the
contribution of primary and fluorescent radiations
JOURNAL OF ANALYTICAL CHEMISTRY Vol. 66
1061
scattered by the sample, the contribution of the pre
excitation of the sample by Auger electrons and pho
toelectrons, the cascade transitions, etc. The possibil
ities of theoretical simulation, previously successfully
used for geological and industrial materials [38], were
studied for coal ash and plants [87]. The calculation
was performed for standard reference samples (SRS)
of coal ash and rocks, and for the ash samples of lichen
and the following plants: alfalfa; potato and sugar beet;
grains of rice, rye, and buckwheat; parts of spinach,
rice, and canola. The analysis of the obtained data
showed a significant effect of the chemical composi
tions of the samples of plant ash and coal on the mag
nitude of the analytical signal Irel. Thus, for plant
materials, Irel for SiKα varies from 1.06 to 1.60; simi
larly, for PKα, from 0.89 to 1.83; for VKα], from 0.46
to 1.15; for FeKα, from 0.51 to 1.33; and for RbKα,
from 0.71 to 2.01. The comparison of the results of Irel
calculated for materials discussed in [87] with the data
for some rock samples revealed the possibility of
selecting SRS with similar values Irel. Note that the
collection of currently available SRS of rocks contains
more than 400 samples, which greatly exceeds the
number of SRS for plant ash and coal. The estimates
for nonashed plant materials [87], showed a significant
effect of the chemical composition of samples on the
intensity of shortwave analytical lines, for example,
FeKα and RbKα in the case of cereals (rice, wheat,
rye, peas, corn, barley, oats), Irel changed by 19–20%,
while for hay and straw (rice, wheat, rye, corn, barley,
oats, alfalfa, soybeans, sunflowers, vetch, timothy, clo
ver, etc.) by 67–69%. Similarly, for SiKα the intensity
changed by 2.2 and 8.5%, respectively; while for nitro
gen, the intensity of NKαline, in the range of only 3–
5%.
Using the theoretical values of intensity, Molcha
nova, Smagunova, and Smagunov [88, 89] investigated
the problem of accounting for the dependence of α
coefficients in the equations of Lachance or Tertiane–
Claisse in the XRF analysis of multicomponent mate
rials. Their conclusions are based on the estimates of
the errors in the determination of chromium in sam
ples similar to steels of various compositions. The
investigations led to the recommendation to calculate
αcoefficients in relation to a multielement sample
and to approximate function α = F(c) in a real range of
variations of ci and cj. The theoretical intensities of
analytical lines were used in the selection of the
approach for accounting the mutual effects of ele
ments for the case of the determination of arsenic in
the soil dumps of the processing of Co–Ni ores in the
plant Tuvakobalt [90]. It was shown that the standard
samples of background should be used to ensure an
acceptable error in the determination of arsenic. At an
early stage of the development of the XRF procedure
for the apatite concentrate, Talanova et al. [91] esti
mated theoretically the value of the mutual effects of
elements. The calculation of intensities was made for
No. 11 2011
1062 REVENKO
the version with the excitation by monochromatic
light. The authors concluded that the mutual effects of
elements should be considered in the determination of
the concentrations of calcium. Possible applications of
the theoretical intensities for similar purposes are pre
sented in [92, 93].
Study of the spectral composition of the Xray
background and its dependence on the chemical com
position of samples. Currently, the main components
of the Xray background for wavelengthdispersive
spectrometers are studied rather thoroughly [35, 38,
39]. Perhaps, this is why only a small number of papers
published in the period under review, is devoted to this
important factor [94–103].
Belykh et al. [96] estimated the contribution of the
primary radiation of the source, multiply scattered by
the atoms of a sample, to the background intensity in
the shortwavelength Xray spectrum in the Xray
radiometric analysis. The estimates were made for the
radioisotope sources Cd109, Am241, Gd153, and Co57
(energy range from 22 to 123 keV) and for the samples
of different chemical composition. It was established
that the maximum of the spectral distribution of mul
tiply scattered radiation is in the area of radiation
incoherently scattered by the sample. Smagunova et
al. [97] experimentally investigated the dependence of
the intensity of the Xray background in the wave
length range of 0.065–0.85 nm on the particle size
(15–360 μm) of single and multiphase systems.
Bolormaa [98] studied the dependence of the intensity
of the Xray background in the wavelength region of
0.06–0.15 nm on the chemical composition of the
solutions deposited on filter paper. It was confirmed
that the main components of the background in the
studied area is the bremsstrahlung of the Xray tube
scattered by the sample and the diffuse scattering of
the characteristic radiation of the elements of a sam
ple.
A number of papers are devoted to the problem of
the formation of the background of energydispersive
apparatus in the longwavelength region of the Xray
spectrum [99–103]. The main difference between the
ratio of individual components of the background in
the cases of energydispersive equipment and crystal
diffraction apparatus is due to the absence of a crystal
analyzer. Consequently, there is neither the contribu
tion of the diffuse scattering of radiation on the crystal
nor the selffluorescence of atoms in the crystal. How
ever, the role of components related to the processes in
the detector significantly increases. The role of the lat
ter factors are especially important in the longwave
length region of the Xray spectrum.
Methods of analysis. Much attention is paid to
assess the boundaries of application and to improve
the conventional methods of analysis that enable the
consideration of the effect of the chemical composi
tion of a sample: the internal standard method [104–
106], the standard background method [107–115], the
method of theoretical corrections [62, 116–123], the
JOURNAL OF ANALYTICAL CHEMISTRY
method of fundamental parameters [124–133], and
the method of constraint equations [4, 134–136].
In the journal Zavodskaya Laboratoriya (2004, no.
6), an article of Il’in was published for discussion
[137]. Its author offered a new (alternative) approach
to XRF, based on the use of the intensity ratios of spec
tral lines of the components of the sample as an ana
lytical signal. Basing on the proposed approach, a pro
cedure for rapid diagnosis of steel and ferrous alloys
was developed. In principle, the elements of such a
solution is widely used in analytical practice. However,
the second part of the work, which contains a “univer
sal version” of the calculation of mutual effects of ele
ments, raises questions and objections. A particular
case of the approach proposed by Il’in—the internal
standard method—has already a number of known
limitations. The main of them are set out in the classi
cal work of Glocker and Schreiber [138]. Borisov and
Fogel’ [139] noted a significant change in the intensity
ratio of the compared SiKα and SrLα lines in the pres
ence of high concentrations of phosphorus in the test
samples. Thus, in the transition from the sample with
a ratio of Si : Sr : P equal to 1 : 2 : 0 to the sample with
the ratio of these components of 2 : 4 : 1, the authors
recorded a decrease of the intensity ratio SiKα/SrLα
by 20%. The conclusion was the following: “Thus, for
quantitative Xray analysis, it is not enough to have a
universal calibration curve for the transition from the
intensity ratio of reference lines to the concentration
of this element in the test mixture. In each case, it is
necessary to know the composition of the object and
the impurities interfering with the determination and
to find a relationship for the transition from the rela
tive intensities of the reference lines to the concentra
tion of the analyte element in the mixtures containing,
in addition to the analyte, the interfering impurities
occurring in this sample.” The detailed investigations
of the errors of the internal standard method were per
formed in the works of Losev and Smagunova [104,
140–143].
One of the objectives of the analyst is to find sim
pler solutions for a specific test material. These solu
tions are usually based on a study of the variations of a
chemical composition of the material. Note that
under certain conditions, even the external standard
method can provide an acceptable accuracy of analysis
for materials with wide ranges of the concentrations of
affecting elements. In some cases, a correlation
between the concentrations of individual elements can
reduce the spread of points around the calibration
curve. It is important that in the development of a pro
cedure, the limits of its applicability should be clearly
defined. Sometimes, a particular solution is notable
for its simplicity and logic. In this case, it appears that
the author of [137] was somewhat carried away by the
found solutions, and this caused the proposition like:
“This opens up new possibilities for quantitative XRF
analysis” (p. 10 of the cited article). In this publica
tion, namely this conclusion raises an objection. A
Vol. 66 No. 11 2011
 DEVELOPMENT OF XRAY FLUORESCENCE ANALYSIS
critical consideration of the proposal of Il’in on the
use of atomic concentrations [144–148] can be found
in the work of Pavlinskii [149].
Ivanenko et al. [150, 151] investigated the depen
dence of the mutual effects of elements on the atomic
number of the interfering element in energydispersive
XRF. As a result, they approximated this dependence
for the elements from potassium to bromine (in this
case, the effects of three elements with lower Z and the
five elements with higher Z was taken into account).
The authors used such an approach in the study of
oceanic nodules. Kos’yanov [152, 153] proposed the
use of an additional absorber for the material of the
sample. The approach is applicable for both quantita
tive Xray fluorescence and Xray diffraction analysis.
The author found the optimal conditions for the use of
auxiliary absorbers enabling a more complete account
of the effect of the filler for particular cases of analysis.
Preparation of samples for analysis. The features of
this important stage of analysis were discussed in sev
eral reviews and monographs [1, 4, 13, 26, 30, 38, 39,
154–156]. The general scheme of the preparation of
emitters from the rock materials for XRF is presented
in monograph [38]; a detailed overview of this phase of
XRF is given in [157, 158], and the features of individ
ual methods of sample preparation for natural materi
als, including rocks, are described in [156]. The prob
lems and prospects of XRF of heterogeneous powder
materials, as in the late part of the 20th century, are
considered in detail by Duimakaev et al. [155]. The
impact of the pretreatment of samples on the accuracy
of analytical data is assessed by Aisueva et al. [159].
The options for accounting changes in the mass of a
sample during alloying are reviewed in [160, 161]. The
effect of the conditions of sample preparation for XRF
on the effect of microadsorption heterogeneity was
investigated by Smagunova et al. [162]. Finkel’stein et
al. [163, 164] and Smagunova et al. [165] attempted to
theoretically describe the intensity of Xray fluores
cence and of the scattered primary radiation on the
particle size in the XRF analysis of powder and pulp
samples.
The possibility of using the volumetric dosing in the
homogenization of some silicate materials is consid
ered in [166]. The procedures for determining the
concentrations of individual elements with precon
centration are described in [167–173]. A simple and
reliable procedure of making reference samples for
XRF is described by Titarenko et al. [174]. During the
considered period, several original methods for pre
paring samples for XRF analysis were patented [175–
177].
The standard version of making an emitter for
TXRF supposes the obtaining of thin samples. This
eliminates the problem of mutual effects of elements.
In the case of a liquid sample, a fixed quantity is
applied by a pipette to the reflector and dried. Such a
method is inacceptable for the samples, for which the
drying is impossible, or when a part of the sample
JOURNAL OF ANALYTICAL CHEMISTRY Vol. 66
1063
components become volatile during drying. It should
be remembered about the problem of representative
ness, which becomes more complicated when dealing
with small portions of materials [23, 141]. As in the
general case of XRF, grinding, abrasion, or dissolution
are usually recommended for homogenizing heteroge
neous samples [38, 141, 178].
XRF with total external reflection. The principle
Xray fluorescence analysis with total external reflec
tion (TXRF) is that in the falling of the primary radia
tion to the substrate with a sample under a very small
angle (0.3–0.6°), it reflects by the atoms of the top
layer of the emitter due to the effect of total external
reflection [2, 24–26, 38, 178]. A part of the radiation
of the primary beam is absorbed by the atoms of the
test sample deposited as a thin layer of a special reflec
tor. The characteristic fluorescent radiation from the
sample is recorded by a semiconductor detector. The
detector is placed above the sample. In this version, the
detector records mainly fluorescent radiation. If, in
addition to this, the primary radiation becomes mono
chromatic, for example, using multilayer crystals, then
a very low background level is obtained for the
recorded spectrum. The spectrum for the whole range
of the determined elements, for example, from Na or
Al to U, is recorded simultaneously. The theoretical
foundations of TXRF are described in detail in numer
ous articles and reviews; the apparatus are available;
and the advantages and disadvantages are clear.
The possibilities of using the XRF version with total
external reflection for the study of geological samples
are examined in review [26]. The historical stages of
the development of instrumental base and method
ological support, sample preparation, and quantitative
analysis are discussed. The applications of TXRF in
the assessment of the environment, in biology, in the
control of pollutions of semiconductor materials, in
the study of cultural values, etc. are exemplified. The
main attention has been paid to the possibilities of
studying geological samples, such as natural waters,
soils and sediments, and rocks, by using TXRF.
Russian researchers were involved in the works on
the application of mainly this variant of XRF [167–
169, 179–199]. Note here the original works of Egorov
et al. on the application of planar waveguides [179–
182]. The idea of planar waveguides is also used in a
number of later works of foreign authors, in particular,
[200, 201].
Pavlinskii, Smagunova, et al. [191] estimated the
errors in the determination of individual elements by
TXRF, caused by various factors.
Practical application of XRF. The situation in Rus
sia at the turn of the century with the development and
production Xray spectral equipment is adequately
described in the works of Revenko, Afonin, Komya
kov, Brytova, Mezhevich, and others [7, 35, 202, 203].
A significant expansion of the applications fields of
XRF in recent decades is due to a sharp increase in the
number of Xray facilities and the improve in their per
No. 11 2011
1064 REVENKO
formance, a more efficient use of modern computers
in XRF, a significant improvement in performance of
semiconductor detectors with thermoelectric cooling,
the development and use of facilities based on total
external reflection of Xray (TXRF), and the use of
capillary Xray waveguides and the development on
their basis of a new version of XRF, that is, microXRF.
The works of the group headed by Kumakhov on cap
illary optics can be highlighted among the achieve
ments of the Russian scientists [9, 10, 14, 20]. The
physical and technological principles of capillary
optics have been proposed and developed in Russia in
the mid1980s. Currently, several versions of Xray
spectrometers using polycapillary lenses are produced
in low volumes. In Russia, these are a “Focus2” spec
trometer with a focal spot of approximately 100 μm
[204, 205], an MKh10 microfocus Xray fluores
cence spectrometer with a focal spot of about 10 μm
(Institute for Roentgen Optics, Moscow, http://
www.xrayoptic.ru/), and an XArt M with a focal spot
of 100 μm and more (Comita, St. Petersburg, www.
comita.ru/projects/x_art_universal_analyzer/) [206].
The study of rocks, soils, and sediments. The appli
cation of XRF for the investigation of geological spec
imens is one of its traditional tasks. Russian research
ers have made and make a significant contribution to
solving this analytical problem. The results are sum
marized in the reviews, monographs, and articles,
where specific options of the applied analysis tech
niques are discussed [13, 15, 27, 31, 32, 35, 38, 39, 61,
72, 74, 110, 111, 115, 120, 121, 124, 125, 128, 154,
156, 164, 207, 208]. All this has led to the fact that
XRF is currently used in studies of materials from both
the bottom of the sea and the lunar surface (a Rifma
(Rhyme) spectrometer on the lunar rover) and the
Mars surface. Borkhodoev proposed to systematize
the problems of the quantitative XRF analysis of rocks
with the following criteria: the significance of the con
tribution of individual elements to the matrix effects,
the relative positions of the characteristic lines of the
Xray spectrum of elements on a scale of wavelengths,
the resolution power of the Xray spectrometer, and
geochemical bonds and the abundance of elements in
various rocks [208]. Elements, the joint determination
of which presumably provide the best accuracy of the
analysis, are combined within one task.
Gunicheva and Aysueva published a series of works
on the XRF analysis of soil [159, 210–214]. The
degree of agreement between the domestic SRS of
soils and their consistency with the SRS of the series
GSS (China), as well as the compliance of the former
with the requirements of the first international project
on global geochemical mapping are evaluated in [159].
The procedure for the nondestructive XRF determi
nation of major elements and S, Ba, Sr, and Zr was
developed for soils, sediments, silts, and loose sedi
ments [209, 210]. The procedure for considering
mutual effects of the elements was based on αfactors
calculated for homogeneous materials (an SRM25
JOURNAL OF ANALYTICAL CHEMISTRY
spectrometer). The authors of [212] studied the effect
of the chemical composition and the concentration of
organic matter for soils and proposed the method for
accounting these factors in the XRF analysis of
humated and geochemically contrasting soils.
The scope of this review leaves out the detailed dis
cussion of the individual achievements of recent works
on the application of XRF in geology. Nevertheless, I
consider it necessary to acknowledge the contribu
tions of the authors of [215–225]. Interesting results
were obtained by Chubarov and Finkel’stein [223–
225] on the determination of FeO/Fe2O3tot by the K
series of the Xray fluorescence spectrum in igneous,
metamorphic, and sedimentary rocks and in iron ores.
The authors took the recommendation of Filippov et
al. [226] as the basis.
A great deal of research of samples of rocks, soils
and sediments was carried using a synchrotron
(Novosibirsk). Unfortunately, a typical mistake that
appears in publications produced by the results of
measurements on this synchrotron is the ignoring of a
widely accepted approach to describe the features of
the methods of analysis used by the authors. Some
times, the information about the details of specific
methods of analysis is completely absent. It was
already noted in [21, 23, 156]. The external standard
method is expected to be applied in the cases of thin
samples and the samples that are close in chemical
composition. It should be noted that very often this
method is applied without any justification or verifica
tion. Some authors have ignored the recommenda
tions on the application of conventional methods of
XRD, worked out by previous generations of research
ers. The method of fundamental parameters is not
always correctly applied. For example, it was applied
very often in the cases of heterogeneous samples,
although the relations valid for homogeneous samples
are used. It is clear that such an attitude is unaccept
able for solving fundamental geological problems.
Plant materials. Biology and Medicine. A rather
detailed consideration of the application of XRF for
the investigation of plant materials can be found in
[87, 227, 228].
The data on the use of Xray diffraction to solve
some problems of biology and medicine are presented
in reviews [7, 229]. During the period under review,
the results of the determination of the major and trace
elements in red cell mass, serum and whole blood,
human hair, tooth enamel, and the tissues of the thy
roid gland have been published. Some authors note
that they have to develop special procedures for each
type of biological materials (blood, bone, kidney and
liver, hair). In the works of our Russian colleagues,
wavedispersive spectrometers (VRA30, Pioneer, and
others), total external reflection spectrometers, and
synchrotron radiation XRF (SRXFR) are used to
study biological materials. Savchenko et al. [230] note
that the collection of hair for analysis causes no
trauma and eliminates the risk of infection. The col
Vol. 66 No. 11 2011
 DEVELOPMENT OF XRAY FLUORESCENCE ANALYSIS
lecting of hair is simple; the samples are easily trans
ported and stored and are suitable for mass research.
The blood and hair samples of tundra Nenets people
were collected in an expedition (1996) [230]. The
blood samples were collected directly in the camps and
brigades and were transported by a helicopter to a field
laboratory within 6 h after collecting. A sample of
packed red blood cells, obtained after centrifugation
and separation of plasma and a lymphocyte layer, was
prepared by applying 20 μL on a Whatman filter
(1 cm2). The samples were dried on air and placed
between two layers of a Teflon film stretched in a
Teflon hoop. Hair was cut into small pieces with stain
less steel scissors, washed successively with acetone,
distilled water, and again with acetone. Next, the sam
ples were dried between two paper filters, and then
pressed into pellets 1 cm in diameter and 20–40 mg in
weight. In another experiment, an additive of polyeth
ylene in a ratio of 1:1 was used in the pressing. The
concentrations of the following elements were mea
sured: Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As,
Se, Br, Rb, Sr, Y, Zr, Mo, W, Hg, Pb, Th, and U. These
investigations can serve as a basis for studying environ
mentallyrelevant relationships of human populations
and its habitat. To excite fluorescence, Kolmogorov et
al. [231] used Xray radiation monochromatized with
a toroidalshaped crystal of pyrolytic graphite, cut
according to the Johann scheme. The fluorescent
radiation of analyte elements was recorded with a
Si(Li) detector from ORTEC. The achieved detection
limits for several elements (Zn, Se, Br, Sr, Hg, and Pb)
were less than 1 μg/g.
Among the work of the last decade, a series of works
of Gunicheva and Pashkova [232–241] should be
noted for the study of the possibilities and the develop
ment of a procedure for determining the concentra
tions of trace elements in milk. The features of the
XRF determination of the concentrations of trace ele
ments in milk and dairy products are described in the
review [240]. Much attention is paid to the informa
tion on the equipment for XRF, the methods of sample
preparation, and the obtaining of calibration curves.
Some examples are given on the use of XRF for study
ing the products of the dairy industry and cow and
human milk.
Industrial applications. The procedure of Xray
rapid analysis of fluorite applied as an initial compo
nent for blending in the technology of slagforming
mixtures was developed [242]. The practice of using an
SRM25 spectrometer for solving the problems of
production control is set out in the following articles:
Mikhailova [243] (the analysis of roll cast in express
laboratory);
Mandrygin et al. [244, 245] (six spectrometers at
the West Siberian Metallurgical Plant; the products of
the domain, converter, and oxygenconverter plants);
Soboleva et al. [246–248] (the development of the
procedures for analyzing slagforming mixtures, low
JOURNAL OF ANALYTICAL CHEMISTRY Vol. 66
1065
carbon ferrochrome, and nickel monoxide at Mechel
JSC);
Kondratyuk et al. [249] (quality control of vana
dium products at Uralredmet JSC).
Kutvitskii et al. [250] used a VRA30 spectrometer
for the determination of Dy, Ti, Nb, and Zr in doped
dysprosium titanate; for the same spectrometer,
Smirnov and Talanova developed the procedures for
determining the concentrations of the main substance
and impurities in the production of pure strontium
compounds [251]. The procedure for the Xray deter
mination of nickel in blister and anode copper with the
use of induction melting was developed by Krasavin et
al. for an ARL72000 spectrometer at MMC Norilsk
Nickel [252]. Lomakina et al. proposed a procedure
for determining the concentration of some elements in
ferrotitanium and ferromolybdenum [253] with the
use of an ARL72000 spectrometer. Namestnikova et
al. [254] developed procedures for determining the
concentrations of a large group of elements in the cop
perbased alloys, using an ARL 9800 spectrometer
(prior to 2003, CPM25 was successfully used for this
task at Severstal JSC).
Trubachev et al. [255] showed that a KRAB
ZOOM Xray analyzer could be used to determine the
elemental composition of the wear products of metal
surfaces and to assess their durability. To obtain the
thin layers of the particles of the test material on the
surface of abrasive paper, a sampling device with the
dosage load on the abrasion surface was proposed. The
authors investigated the wear of the Cu–Mo coatings
with the use of the data of electrochemical determina
tion.
The determination of the thickness and elemental
composition of coatings and thin films by XRF was
discussed in [198, 199, 256–259]. A set of methods for
determining impurities in multisilicon and in the
products of its production process is described in
[260], while an example of the successful application
of energy dispersive XRF for a forensic study of three
component jewelry gold alloys is given in [261]. A
number of papers present the procedures for the inves
tigation of petroleum and petroleum products [262–
264] and lubricating oils [265–268] in the engine wear
products. The possibilities of continuous monitoring
of ironore blends were considered by Alov et al. [269,
270]. Kitov and Mukhachev [271] described an origi
nal version of the separation of particles by fractions
with known elemental composition of these particles.
The results indicated that this problem was success
fully solved in that case when the separated fractions
were considerably different in the absorbing and scat
tering characteristics for the Xray radiation incident
on the sample.
Samples of the cultural heritage. A.G. Revenko and
V.A. Revenko reexamined the features of the applica
tion of XRF for studying materials of cultural heritage
[272–275]. The potential of Xray spectral analysis
and a large number of researchers have provided the
No. 11 2011
1066 REVENKO
method with a wide application in the study of these
objects. In the literature, one can find the examples of
the application of XRF for the investigation of art
objects such as paintings on glass, various utensils,
ornaments, etc. The work of an analyst in the study of
these materials is similar to the work of a criminalist.
In both cases, it is necessary to restore the picture of
what happened and how, using the tiniest bits of pre
served material. The found material is desirable to pre
serve. Probably for these reasons, one of the sections of
the annual reviews in the Journal of Atomic Absorption
Spectrometry is devoted to the discussions of the appli
cation of XRF in archeology and forensic science
[276]. Another circumstance is of particular impor
tance: the results of the work serve as a basis for the
conclusions, on which the fate of people (in forensic)
or ideas (from analysts who study the materials in
question) depend. Therefore, it is very important to
get real results.
Kalinin and Taganov developed a technique for
determining the concentrations of carbon and applied
it in the examination and the attribution of the Indo
Persian damask arms of the XVII century [277]. A
FocusM spectrometer was developed at the Institute
for Roentgen Optics (IRO, Moscow) by Shcherbakov
et al. [205, 206]. It is equipped with an Xray tube with
a Mo anode with a capacity of up to 50 W and with a
polycapillary lens with a focal spot size from 50 to
300 μm. The test area is selected using an optical
microscope. The sample can be moved in three direc
tions; the minimum distance between the sample and
the detector is 10 mm. In the Tretyakov Gallery, the
icon of Andrei Rublev Troitsa (Trinity) and a series of
paintings by Russian avantgarde artists, including
Marc Chagall, Udaltsov, and others were examined
with the use of a microXRF spectrometer [278]. The
same spectrometer was used by Esposito et al. [279]
from the National Laboratory of Frascati (Italy) for
the study of antique items of terracotta and other
ceramics. The potential of the prototype of this device
for the study of materials of cultural heritage was dis
cussed by Benedetti et al. [280]. They, in particular,
analyzed the samples from the walls of an ancient
underground water tank and the fragments of frescoes
of Palazzo Maggi by Pompiano.
The results of the theoretical evaluation of the
mutual influence of elements in the XRF analysis of
some types of glass are presented in [281]. The findings
showed that this factor should be taken into account:
for the test samples, the relative specific intensity (Irel)
of analytical lines for some elements varied by 2–
5 times in going from antique glass and obsidians to
the samples of mosaic glass or iridescent glass.
Erusalimchik et al. assessed the possibility of an
EAGLEII microXRF spectrometer with the pri
mary beam diameter of ~100 μm for the study the cor
rosion of silver coins [282, 283]. The obtained results
allowed the authors to find out the causes of corrosion
JOURNAL OF ANALYTICAL CHEMISTRY
and to develop recommendations on the chemical
composition of such coins.
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