ARTICLE IN PRESS

Radiation Physics and Chemistry 75 (2006) 7–13

www.elsevier.com/locate/radphyschem

Non-validity of Bragg’s additivity law for rare-earth

compounds
B.R. Kerura,, M.T. Lagarea, R. Nathuramb
a
Department of Physics, Gulbarga University, Gulbarga 585 103, India
b
Radiation Safety Systems Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085, India
Received 12 January 2005; received in revised form 22 February 2005; accepted 22 February 2005

Abstract

Mass attenuation coefficients have been measured for rare-earth compounds at averaged photon energies 5.947 and
8.118 keV. The measured values are compared with theoretical calculations. The disagreement between experiment and
theory is larger than the experimental error when the incident photon energy is close to the L shell absorption edge.
Further away from the edge the agreement between experiment and theory is within 3%. The breakdown of the mixture
rule close to L absorption edges is discussed.
r 2005 Elsevier Ltd. All rights reserved.

1. Introduction where Ai is the atomic weight of the ith element, and ai is

The mass attenuation coefficient, m/r, for any
chemical compounds is usually estimated from the sum
of the weighted contributions of the constituent
elements. The underlying assumption is that these
contributions are additive, a law known as Bragg’s
additivity law or, more commonly, the mixture rule. It
can be formulated that


m X m
¼ wi , (1)
r i
r i
where (m/r)i and wi are the mass attenuation coefficient
and the fraction by weight, respectively, of the ith
element. For a chemical compound, wi can be written as
ai Ai
wi ¼ P , (2)
aj Aj
j that current methods of calculations are inaccurate at
Corresponding author.
E-mail address: kerur_vrk@yahoo.com (B.R. Kerur).
the number of formula units in the compound.
The X-ray transmission, T, is defined as
T ¼ I=I 0 , (3)
where I and I0 are the observed intensities with and
without absorber.
The mixture rule ignores any changes in the atomic
wave functions as a result of the molecular, chemical and
crystalline environment (Jackson and Hawkes, 1981). As
pointed out by Deslattes (1969), errors in the estimation
of the m/r for compounds are generally less than a few
percent at photon energies more than 1 keV away from
any absorption edge. According to Jackson (1982), the
validity of the mixture rule is not well established in the
soft X-ray region and in particular close to absorption
edges, where chemical effects may give rise to a break-
down of the mixture rule. Jackson (1982) also points out
photon energies near any absorption edge and that
experimental evidence of chemical effects is needed.
Similarly, Lakshminarayana (1984) has stressed the need

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doi:10.1016/j.radphyschem.2005.02.009
 ARTICLE IN PRESS
8 B.R. Kerur et al. / Radiation Physics and Chemistry 75 (2006) 7–13
for accurate determination of total or partial cross
sections to check the validity of the mixture rule. First
experimental results were presented by Deslattes (1969)
for sulphates. Later, Lakshminarayana et al. (1986) and
Tan et al. (1988) measured photon cross-sections near
the Br K edge. Chemical effects indicating the non-
validity of the additivity law were found for energies up
to 1 keV above the edge. Similarly, Kerur et al. (1991,
1992, 1993, 1994) have thoroughly studied photon cross
sections at or near absorption edges and shown that
deviations from the mixture rule occur as far as 1.2 keV
above the edge, and also some 42 eV below the edge for
transition elements.
Manson (1989), Gerward (1993) and Hubbell (2000)
have stressed that although photo ionization has been
studied experimentally and theoretically for more than
half a century, accurate results are rare, particularly at
low energies. As pointed out by Saloman et al. (1988),
the quality of the experimental data, and thus our
knowledge of absorption cross sections, degrades with
decreasing energy as well as near edges (thresholds),
emphasizing the need for accurate experimental data.
The present investigation has two aspects. First, we
have selected compounds whose absorption edges are
far away from the incident photon energy in order to
compare our experimental results with calculated m/r
values using the mixture rule. The expected agreement
between experiment and theory will confirm the validity
of the mixture rule as well as the usefulness of our
experimental method. Next, we have chosen com-
pounds, the absorption edges of which are close to the
incident photon energy. Any discrepancy between
experiment and theory will then point to the non-
validity of the mixture rule. Due to limited resources and
facilities, the problem was not tackled directly by
varying the incident photon energy. Instead we have
adopted the alternate method of keeping the incident
photon energy constant and varying the absorption edge
energy (Eb) by selecting suitable compounds. Hence, we
are studying the variation of m/r as a function of atomic
number, Z, rather than of incident photon energy, Ex.
In the present measurement, the validity of Bragg’s
additivity law is studied near the L edges of some rare-
earth compounds. The selection of compounds was
dictated by the incident photon energy and by the
availability of thin foils. We have used 55Fe and 65Zn
radioactive X-ray sources with weighted average Kab
energies 5.947 and 8.118 keV energy, respectively. The
rare-earth compounds represent elements with atomic
numbers in the region 57pZp70.
2. Experimental
The experimental configuration is the same as in a
previous work (Nagabhushan et al., 2004). A rigid stand
positioned above the detector holds the source, specimen
and collimator in place and ensures vertical alignment.
Photons from the radioactive source are collimated by
an aluminum collimator and are incident on the
specimen foil positioned normal to the beam and
midway between source and detector. Photons passing
through a second aluminum collimator are detected by
an NaI(Tl) crystal. To reduce the background of
scattered radiation, the stand is made of Perspex, and
a mild steel plate is placed above the detector. The
thickness of each collimator is 1.2 cm, adequate for the
energies involved.
Radioisotopes of 55Fe and 65Zn were deposited over
an active area of 10 mm diameter between two mylar
films, held in a Perspex ring of 25 mm diameter. Sources
with a strength of about 20 mCi were procured from
BRIT, Mumbai, India. 55Fe decays by electron capture
to the ground state 55Mn, emitting Mn Ka1, Ka2 and Kb
characteristic radiation with energies 5.899, 5.888 and
6.490 keV, respectively. Another source, 65Zn, decays
by electron capture partly to an excited state and partly
to the ground state 65Cu, and also by positron emission
to the ground state 65Cu, emitting Cu Ka1, Ka2 and Kb
radiation with energies 8.048, 8.028 and 8.905 keV,
respectively, and 1115 keV gamma rays.
Because of the low resolution of the detector, only one
photo peak is observed for each source. The weighted
average energy of Ka and Kb, taken in the ratio 70:6.75
(as calculated from the intensity within the FWHM of
the photo peak) is 5.947 keV for 55Fe source and
8.118 keV for 65Zn source (Kerur et al., 1991). No
noticeable impurities were found in the photon spectra.
The inner bremsstrahlung intensity from the sources was
found to be negligible compared to the X-ray intensity in
the region of interest. The background counts and the
contributions from the radiations other than the X-rays
of interest were determined in an elaborate way,
depending on the type of source employed. Details have
been discussed elsewhere (Kerur et al., 1991; Nagab-
hushan et al., 2004).
Nine rare-earth sulphate compounds were chosen,
covering a wide range of atomic numbers: La (57), Pr
(59), Nd (60), Sm (62), Eu (63), Gd (64), Tb (65), Dy (66)
and Yb (70). The compounds were purchased from
Indian Rare Earths Ltd., Udyogamandal, India, with
purity between 99.90% and 99.99%. Details of the rare-
earth compounds are presented in Table 1. At the
photon energies considered, the sample thickness
required to cover the transmission range 0.5XTX0.02
would be very small, of the order of a few mg/cm2.
Although various techniques to prepare thin foils are
mentioned in the literature, our laboratory does not
have the necessary facilities. Hence a simple but effective
method was adopted: the blotting paper method (Kerur
et al., 1993) where a solution of known concentration is
deposited on good quality blotting paper. The method is
 ARTICLE IN PRESS
B.R. Kerur et al. / Radiation Physics and Chemistry 75 (2006) 7–13 9

Table 1 uniformity, as a precaution. To increase the mass

Chemical formulas and L absorption-edge energies of rare- thickness, the normality of the solution was increased
earth compounds and the procedure was repeated. Samples of different
thickness, covering the desired transmission range,
Compound Z EL (keV)
were obtained by stacking together the required number
La2(SO4)3  9H2O 57 LI:6.266 of foils.
LII:5.891 The X-ray spectrometer consisted of a Bicron (USA)
LIII:5.483 Model 1xM.040/2B X-ray detector with a rated resolu-
Pr2(SO4)3  8H2O 59 LI:6.835 tion of 55% at 5.0 keV and an Oxford Instruments Inc.
LII:6.440 (USA), Model PCA-P, multi-channel analyzer (MCA).
LIII:5.964 The 1 mm thick
25 mm dia NaI(Tl) crystal was
mounted on a 51 mm diameter photomultiplier. Using
Nd2(SO4)3  8H2O 60 LI:7.126 a Windows based software, Oxford Win-MCA, all
LII:6.722
parameters of the X-ray spectrometer could be set, and
LIII:6.208
the spectra recorded and analyzed. The X-ray spectro-
Sm2(SO4)3  6H2O 62 LI:7.737 meter was calibrated using the radioisotopes mentioned
LII:7.312 earlier. The temperature around X-ray spectrometer was
LIII:6.716 maintained at 2671 1C throughout the experiments. The
Eu2(SO4)3  8H2O 63 LI:8.052 long-time stability and linearity of the spectrometer were
LII:7.617 checked before data collection.
LIII:6.977 Photon spectra were recorded in the following
sequence. Spectrum B (background spectrum) was
Gd2(SO4)3  8H2O 64 LI:8.376
LII:7.930
recorded without source and sample. Spectrum BS
LIII:7.243 (background plus source spectrum) was recorded with
the source but without the sample. Spectrum BT
Tb2(SO4)3  8H2O 65 LI:8.708 (background plus transmitted spectrum) was recorded
LII:8.252
with the source and the sample. Spectrum B and
LIII:7.514
Spectrum BS were recorded again. The incident spec-
Dy2(SO4)3  8H2O 66 LI:9.046 trum was obtained by subtracting Spectrum B from
LII:8.581 Spectrum BS and the transmitted spectrum was
LIII:7.790 obtained by subtracting Spectrum B from Spectrum
Yb2(SO4)3  8H2O 70 LI:10.486 BT. The photopeak had a gaussian distribution and
LII:9.978 hence about 70% of the counts under photopeak were
LIII:8.944 contained in the channels within the FWHM.
By integrating the incident spectrum and the trans-
Z is the atomic number of the rare-earth element, and ELi, i ¼ I, mitted spectrum over the selected width of the photo-
II and II, are the L sub-shell binding energies. peak, the incident intensity I0 and the transmitted
intensity I were obtained. Finally, m/r was obtained
as the slope of a straight line fitted to a plot of ln T
simple but very tedious in order to obtain a uniform as a function of mass thickness (in units of mass per
deposition. unit area) by a least-squares method. Prior to analysis
A fine quality Whatman (No. 1) blotting paper was the observed intensities were corrected for the detector
selected and circular foils were cut. The uniformity of dead time.
each foil was checked by X-ray transmission at small Three important parameters have to be carefully
areas of the sample. Only foils that were uniform over selected to get accurate values for m/r. First, the
their entire area were selected for preparing the final collimator has to be narrow enough to avoid scat-
samples. The mass per unit area was measured by a tered radiations reaching the detector, but wide
microbalance and a traveling microscope. A known enough to give a sufficiently high count rate with
amount of solution with known concentration was respect to the counting statistics. Second, the region
deposited uniformly on the selected blotting paper, of interest for integrating the counts in the photopeak
using a calibrated syringe. After evaporation of the has to be chosen appropriately, avoiding counting
solvent, a circular foil of 1.2 cm diameter, was cut by a photons that have suffered small-angle and multiple
punch. Again, its uniformity was tested by X-ray scattering and yet reached the detector. In the pre-
transmission. The mass per unit area was measured, sent work we have adopted the recommendation of
correcting for the blotting paper itself. Before data Kerur et al. (1991) to consider the FWHM of the
collection, all foils were checked once more for photopeak for integration. Third, the transmission
 ARTICLE IN PRESS
10 B.R. Kerur et al. / Radiation Physics and Chemistry 75 (2006) 7–13

Table 2
Mass attenuation coefficients of rare-earth compounds at 5.947 keV

Compound DE (keV) Experimental value (cm2/g) Theoretical value (cm2/g) PD (%)

La2(SO4)3  9H2O 0.319 240.073.5 287.1 WinXCom 16.

+0.056 289.9 HS
+0.464

Pr2(SO4)3  8H2O 0.888 110.772.5 116.2 WinXCom 4.7

0.493 119.5 HS
0.017
Nd2(SO4)3  8H2O 1.179 125.872.7 120.5 WinXCom +4.4
0.775 124.4 HS
0.261
Sm2(SO4)3  6H2O 1.790 134.271.9 135.0 WinXCom 0.6
1.365 133.9 HS
0.769
Eu2(SO4)3  8H2O 2.205 133.671.7 135.0 WinXCom 1.0
1.670 138.9 HS
1.030
Gd2(SO4)3  8H2O 2.429 138.171.9 139.4 WinXCom 0.9
1.983 142.4 HS
1.296
Tb2(SO4)3  8H2O 2.761 143.272.1 145.0 WinXCom 1.2
2.305 144.7 HS
1.567
Dy2(SO4)3  8H2O 3.099 152.272.8 150.1 WinXCom +1.4
2.634 151.4 HS
1.843
Yb2(SO4)3  8H2O 4.539 173.272.1 174.3 WinXCom 0.6
4.031 175.4 HS
2.997

DE ¼ ExELi, where i ¼ I, II, III; HS ¼ Hubbell and Seltzer, 1995.

range, chosen for linear regression and determination of

m/r, should be such that Lambert-Beer’s law is
rigorously valid. Nagabhushan et al. (2004) have
suggested the transmission range 0.02pTp0.5 when
using the FWHM for integration.
Using the experimental parameters as stated above,
we have determined m/r for the selected rare-earth
compounds. The incident intensity was found by
determining the intensity with a dummy blotting paper
foil at the sample position. The transmitted intensity of
X-rays for various specimen thicknesses was recorded
and appropriate corrections were made. Then a plot of
the logarithm of transmitted intensity as a function of
sample thickness was made and the m/r value was
calculated using only those points which were suffi-
ciently close to the least-squares fit in the transmission Fig. 1. The mass attenuation coefficient m/r of rare-earth
region mentioned above. For each specimen, m/r was compounds at 5.947 keV as a function of atomic number Z.
determined two–three times to ensure a reproducibility Filled symbols are experimental data points, and open symbols
within 2% for all samples. are calculated values.
 ARTICLE IN PRESS
B.R. Kerur et al. / Radiation Physics and Chemistry 75 (2006) 7–13 11

Table 3
Mass attenuation coefficients of rare-earth compounds at 8.118 keV

Compound DE (keV) Experimental value (cm2/g) Theoretical value (cm2/g) PD (%)

La2(SO4)3.9H2O +1.852 146.571.0 146.7 WinXCom 0.1

+2.227 148.0 HS
+2.635

Pr2(SO4)3.8H2O +1.283 165.372.3 167.3 WinXCom 1.2

+1.678 164.0 HS
+2.154
Nd2(SO4)3.8H2O +0.992 170.171.8 174.8 WinXCom 2.7
+1.396 171.7 HS
+1.910
Sm2(SO4)3.6H2O +0.381 240.173.0 200.1 WinXCom +20
+0.806 199.7 HS
+1.402
Eu2(SO4)3.8H2O +0.066 159.372.0 199.7 WinXCom 20
+0.501 195.6 HS
+1.141
Gd2(SO4)3.8H2O 0.258 150.272.1 181.7 WinXCom 17
+0.188 178.4 HS
+0.875
Tb2(SO4)3.8H2O 0.590 155.372.1 144.0 WinXCom +7.8
0.134 144.1 HS
+0.604
Dy2(SO4)3.8H2O 0.928 140.172.3 151.0 WinXCom 7.2
0.463 147.4 HS
+0.328
Yb2(SO4)3.8H2O 2.368 79.3171.8 77.67 WinXCom +2.1
1.860 78.35 HS
0.826

DE ¼ ExELi, where i ¼ I, II, III; HS ¼ Hubbell and Seltzer, 1995.

3. Results and discussion

The experimental m/r values along with their asso-

ciated errors, calculated by the least-squares fit, are
given in Table 2, Figs. 1 and Table 3, Fig. 2 for the
photon energies 5.947 and 8.118 keV, respectively. The
theoretical results have been calculated by WinXCom
(Gerward et al., 2001) which is the successor of XCOM
(Berger and Hubbell, 1987/99) using the mixture rule
and theoretical m/r values for the elements. The
percentage difference, PD, between experiment and
theory is also given in the tables together with the
difference, ExEb, between the incident photon energy,
Ex, and the edge energy, Eb. Positive or negative sign
indicate that the edge is below or above the incident
photon energy. Binding energies for the L edges are Fig. 2. The mass attenuation coefficient m/r of rare-earth
from Kortright (1986). Since the reproducibility is about compounds at 8.118 keV as a function of atomic number Z.
2% and the experimental error 3%, a PD less than 5% Filled symbols are experimental data points, and open symbols
should be considered agreement between experiment are calculated values.
 ARTICLE IN PRESS
12 B.R. Kerur et al. / Radiation Physics and Chemistry 75 (2006) 7–13
and theory. A PD greater than 5%, on the other hand,
should be considered as disagreement.
Table 2 shows that there is good agreement between
experiment and theory for the Pr, Nd, Sm, Eu, Gd, Tb,
Dy, and Yb compounds where the values of ExEb are
in the range from –0.017 to 4.539 keV. Similarly, Table
3 shows that there is good agreement for the La, Pr, Nd
compounds with ExEb from +2.635 to +0.992 keV,
and for the Yb compound with ExEb from –2.368 to
0.826 keV. These observations indicate that the mix-
ture rule is valid for compounds having edge energies
0.992 keV or more below, and 0.017 keV or more above
the incident photon energy. The validity of the mixture
rule proves the validity of our method. Thus, our
method is suitable for measuring m/r of any substance,
element, compound or mixture, utilizing any radioactive
X-ray source of pure or mixed type. This gives credence
to our method to measure m/r for compounds the
absorption edges of which are close to the incident
energy on either side.
Table 2 shows that the mixture rule fails by 16% for
the La compound, the LII and LIII absorption edges of
which are 0.056 and 0.464 keV below Ex. On the other
hand, the mixture rule is in agreement with experiment
for Pr with ExEb ranging from 0.888 keV for LI, and
0.493 keV for LII to 0.017 keV for LIII. Table 3 shows
that deviations from the mixture rule by 20, 20, 17,
7.8 and 7.2%, i.e. larger than the 5% uncertainty,
occur for Sm, Eu, Gd, Tb, and Dy, where ExEb ranges
from 0.928 to –0.134 keV, and +0.066 to +0.604 keV
for the LI, LII and LIII edges. In contrast, there is good
agreement with the mixture rule for Yb, where ExEb
ranges from 0.826 to 2.368 keV.
Thus, it is clear that the mixture rule breaks down
near the L absorption edges. In previous work, the non-
validity of the mixture rule was proved up to 1.2 keV
above the K edge (Kerur et al., 1993). In the case of L
edges, the present work indicates that the corresponding
energy range is less than 1.0 keV. The PDs for the rare-
earth compounds of Sm, Eu, Gd, Tb, Dy, may be
attributed to the presence of ‘‘ups’’ and ‘‘troughs’’ in the
fine structure above an edge and demonstrates that the
deviations increase as the edge approaches Ex as
expected from EXAFS studies. Similarly, the non-
validity of the mixture rule is proved within 17 eV below
the edge as evident in the case of the Pr compound. Most
of this deviation may be attributed to Resonance Raman
Scattering (Sparks, 1974; Manninen et al., 1986; Kane
et al., 1987) and in part to impurities and uncertainties in
the photon energy. However, the agreement between
experiment and theory at 8.118 keV, where the L edges
are far below Ex, clearly demonstrates the minor role
played by impurities. Hence, we conclude that contribu-
tions from impurities are negligible in the present case.
The determination of the non-validity of the mixture
rule is complicated by the presence of three edges of the
samples, LI, LII and LIII, and three characteristic lines of
the incident radiation, Ka1, Ka2, and Kb. Hence, there is
an urgent need of conducting further absorption
experiments with strictly monoenergetic photons. This
could be done using synchrotron radiation and a tunable
crystal monochromator. Anyway, the present experi-
mental results indicate, at least qualitatively, the break-
down of the mixture rule near the L edges.
It is important to mention that the theoretical
calculations have been done for single isolated atoms,
and that near the edges these values are extrapolated to
the edge energy. The mixture rule will yield erraneous
estimates for the compounds when using inadequate
theoretical m/r values. Hence, the ‘‘non-validity’’ of the
mixture rule calls for better theoretical as well as
experimental data near L absorption edges. In fact,
the present results demonstrate the existence of EXAFS
and chemical effects (Baydas et al., 1999; Oku et al.,
1999; Takeshi, 2000; Katare et al., 2000; Sogut et al.,
2002) but not necessarily a breakdown of the mixture
rule itself.
Acknowledgments
The authors are highly thankful to Professor L.
Gerward for helpful discussion and encouragement, and
also for providing us with the WinXCom software.
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