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Radiation Physics and Chemistry 75 (2006) 7–13

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

B.R. Kerura,, M.T. Lagarea, R. Nathuramb
Department of Physics, Gulbarga University, Gulbarga 585 103, India
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


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

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

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8 B.R. Kerur et al. / Radiation Physics and Chemistry 75 (2006) 7–13

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

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

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

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.
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

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

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

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.
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, samples, LI, LII and LIII, and three characteristic lines of
should be considered as disagreement. the incident radiation, Ka1, Ka2, and Kb. Hence, there is
Table 2 shows that there is good agreement between an urgent need of conducting further absorption
experiment and theory for the Pr, Nd, Sm, Eu, Gd, Tb, experiments with strictly monoenergetic photons. This
Dy, and Yb compounds where the values of ExEb are could be done using synchrotron radiation and a tunable
in the range from –0.017 to 4.539 keV. Similarly, Table crystal monochromator. Anyway, the present experi-
3 shows that there is good agreement for the La, Pr, Nd mental results indicate, at least qualitatively, the break-
compounds with ExEb from +2.635 to +0.992 keV, down of the mixture rule near the L edges.
and for the Yb compound with ExEb from –2.368 to It is important to mention that the theoretical
0.826 keV. These observations indicate that the mix- calculations have been done for single isolated atoms,
ture rule is valid for compounds having edge energies and that near the edges these values are extrapolated to
0.992 keV or more below, and 0.017 keV or more above the edge energy. The mixture rule will yield erraneous
the incident photon energy. The validity of the mixture estimates for the compounds when using inadequate
rule proves the validity of our method. Thus, our theoretical m/r values. Hence, the ‘‘non-validity’’ of the
method is suitable for measuring m/r of any substance, mixture rule calls for better theoretical as well as
element, compound or mixture, utilizing any radioactive experimental data near L absorption edges. In fact,
X-ray source of pure or mixed type. This gives credence the present results demonstrate the existence of EXAFS
to our method to measure m/r for compounds the and chemical effects (Baydas et al., 1999; Oku et al.,
absorption edges of which are close to the incident 1999; Takeshi, 2000; Katare et al., 2000; Sogut et al.,
energy on either side. 2002) but not necessarily a breakdown of the mixture
Table 2 shows that the mixture rule fails by 16% for rule itself.
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 Acknowledgments
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 The authors are highly thankful to Professor L.
that deviations from the mixture rule by 20, 20, 17, Gerward for helpful discussion and encouragement, and
7.8 and 7.2%, i.e. larger than the 5% uncertainty, also for providing us with the WinXCom software.
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 References
agreement with the mixture rule for Yb, where ExEb
ranges from 0.826 to 2.368 keV. Baydas, E., Sogut, O., Sahin, Y., Buyukkasap, E., 1999.
Thus, it is clear that the mixture rule breaks down Chemical effects on L X-ray fluorescence cross sections of
near the L absorption edges. In previous work, the non- Ba, La, and Ce compounds. Radiat. Phys. Chem. 54,
validity of the mixture rule was proved up to 1.2 keV 217–221.
above the K edge (Kerur et al., 1993). In the case of L Berger, M.J., Hubbell, J.H., 1987/99. XCOM: Photon Cross
edges, the present work indicates that the corresponding Sections Database, Web Version 1.2, available at http://
energy range is less than 1.0 keV. The PDs for the rare- National Institute of Standards and
Technology, Gaithersburg, MD 20899, USA (199). Origin-
earth compounds of Sm, Eu, Gd, Tb, Dy, may be
ally published as NBSIR 87-3597 ‘‘XCOM: Photon Cross
attributed to the presence of ‘‘ups’’ and ‘‘troughs’’ in the
Section on a Personal Computer’’.
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