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Measurement 27 (2000) 43–51

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Requirement of a robust method for the precise determination


of the contact point in the depth sensing hardness test
Christian Ullner*
Federal Institute for Materials Research and Testing ( BAM), Head of Laboratory S.11, 12200 Berlin, Germany
Received 28 July 1998; received in revised form 10 August 1999; accepted 31 August 1999

Abstract

The fundamental quantities in the depth sensing hardness test are force and displacement. The penetration depth used for
the calculation of a certain hardness parameter (for instance HU, Eq. (1)) makes it necessary to determine the contact point.
As shown in the paper, fitting of the force–displacement curve, F(h), by a second order polynomial and extrapolating to
F 5 0 is not always the right way to achieve a sufficiently small uncertainty of depth. The feature of that procedure is
analysed by a simple mathematical model. In dependence of the testing force, the scatter of the experimental data, and the
required limit of depth uncertainty, a profound selection of the fitting range, the fitting function, and the extrapolation
function should be done.  2000 Elsevier Science Ltd. All rights reserved.

Keywords: Instrumented hardness; Uncertainty; Contact point

1. Introduction pyramid and to name the quotient of indentation


force by the contact area of the indenter
The depth sensing hardness test or continuous
indentation test concerns the measurement of force F
HU 5 ]]]]2 (1)
and displacement during the penetration of a pyrami- 26.43(h 2 h 0 )
dal indenter (diamond pyramid) into the material. In
this way the hardness can be determined advantage- as Universal Hardness HU. The divisor is the contact
ously without a human observer. Therefore, this area between indenter and specimen assuming the
method is also named recording or instrumented indenter is a Vickers pyramid with ideal geometry
hardness. (without tip rounding, for instance). The displace-
There are some different definitions for the in- ment difference (h 2 h 0 ) is the actual penetration
strumented hardness. According to the definition by depth into the specimen.
Martens [1] (hardness is the resistance of a solid If HU is constant (homogenous material, no
material against the penetration of a harder material), surface effect, ideal indenter geometry) the universal
Weiler [2] proposed to use a diamond Vickers hardness can be calculated from the slope of the plot
of square-root force against displacement
]
*Tel.: 149-308-104-1914; fax: 149-308-104-1917.
E-mail address: christian.ullner@bam.de (C. Ullner)
]]S D
dŒF 2
dh
HU s 5 ]]]. (2)
26.43
0263-2241 / 00 / $ – see front matter  2000 Elsevier Science Ltd. All rights reserved.
PII: S0263-2241( 99 )00054-8
44 C. Ullner / Measurement 27 (2000) 43 – 51

The determination of the contact point (zero point of


the penetration depth), h 0 , is not needed.
Hardness definitions (1) and (2) given in the
German standard [3] concern both the plastic and
elastic penetration of the indenter. For the determi-
nation of the plastic hardness from the depth sensing
hardness test a model is needed for the actual
penetration depth or for the elastic deformation
around the indentation, respectively. According to
such a model the plastic hardness (in approach to the
conventional Vickers hardness) can be calculated by
the use of the Young’s modulus E [4] or by the use
of the initial unloading slope (dF / dh) F max [5]. Fig. 1. The square root of indentation force plotted against
This paper investigates the uncertainty of in- indenter displacement (Vickers pyramid) for silicon nitride
strumented hardness caused by the determination of ceramics with 3% fine pores (left) and almost free of pores (right,
the contact point, h 0 , in Eq. (1). The precise de- R a 5 0.005 mm). A Fischerscope H 100 with force generating
tection of the contact point is not at all common- system (minimal increment of force 0.02 mN, maximal force 1 N),
depth sensing measurement for the indenter displacement (accura-
place. Additionally, because of the square in the term cy 3 nm), and stepwise incremental force was used. Tests were
(h 2 h 0 )2 , the relative uncertainty of the universal conducted at a data acquisition rate lower than 10 s 21 and a force
hardness is the double value of the relative uncertain- rate, at contact, of 50 mN s 21 .
ty concerning h 0 .

2. Effect of materials and influence of machine

Before the determination of the contact point h 0 is


studied in detail the fluctuations of the force–dis-
placement dependence near the contact point should
be discussed. Typical patterns of the indentation
curves measured repeatedly are shown by silicon
nitride ceramics (HU1512 000 N mm 22 ), optical
glass (HU1054000 N mm 22 ), and steel (HU105
6500 N mm 22 ) in Figs. 1–3. To indicate more
clearly the points of importance for the calculations
done in this paper, the square root of force is plotted
against the displacement and the contact points of the Fig. 2. The square root of indentation force plotted against
curves are selected in such a way that the displace- indenter displacement (Vickers pyramid) for optical glass BK 7
ments of all repeated indentation curves are identical with the roughness R a 5 0.28 mm (left) and R a 5 2.6 mm (right).
A home-made machine with 100 N force transducer (resolution
at maximal force. According to Eq. (2) the slope in
0.5 mN-digits, repeatability 5 mN) and piezotranslator, depth
Figs. 1–3 gives the hardness HU s . Regions of sensing measurement related to the specimen surface (glass scale
straight lines demonstrate the ideal condition of the displacement system, resolution 10 nm-digits, repeatability 50 nm)
constant hardness (the rule of geometric similarity is was used. The tests were conducted at data acquisition rate 10 s 21 ,
valid for homogeneous materials, no surface effects, and penetration rate, at contact, of 50 mN s 21 .
and ideal indenter geometry).
Concluding from Figs. 1–3 which are examples of
the more general investigations on different materials 1. The existence of constant hardness becomes more
at different maximal forces using different machines probable with increasing force. Deviations from
the following points are true. the geometric similarity (blunt indenter tip [6]),
C. Ullner / Measurement 27 (2000) 43 – 51 45

specified hardness definition (Rockwell hardness,


differential hardness, or hardness HU s ). This is not
the objective of this paper. The other alternative is to
accept the significantly high uncertainty contribution
due to the indentation response of the material near
the contact point. Of course, any reduction of the
measuring error gives a more precise determination
of the contact point for an individual indentation test
but the enhanced scatter of repeated indentation tests
caused by various materials response remains, as
indicated by the trumpet shapes in Figs. 1–3.
The objective of this paper is to indicate the
problems occurring with the extrapolation to F 5 0
Fig. 3. The square root of indentation force plotted against for improving the accuracy of the contact point h 0 .
indenter displacement (Vickers pyramid) for steel with the Because the study is done on the individual indenta-
roughness R a 5 0.01 mm (left) and R a 5 0.2 mm (right). A HMO
100R with 100 N force transducer (resolution 5 mN-digits), depth
tion response and the accuracy of the machine allows
sensing measurement related to the specimen surface (LVDT, measuring the certain force–displacement depen-
resolution 5 nm-digit), and continuous force increase was used. dence near the contact point, the study can be limited
The tests were conducted at data acquisition rate 6 s 21 , and to a deterministic model. Only the scatter of force
penetration rate, at contact, of 0.15 mN s 21 . before contact has to be involved.

from the homogeneity of the material (indentation


size effect [7]), and from the well-prepared plan 3. Problems of the extrapolation to F 5 0
surface (effect of roughness [8] and porosity [9])
become more substantial at smaller forces or To determine the contact point h 0 there is an
smaller penetration depth, respectively. obvious way by curve fitting and extrapolation to
2. The scatter of the shape of indentation curves remove the indentation force F. As proposed by
near the contact point is higher than the scatter at Grau et al. [10] the indentation curve is fitted by a
maximal force. It is also higher than the error of polynomial of second order,
the measuring instrument. For this reason, the
distinct scatter of indentation curves near the Fshd 5 a 0 1 a 1 h 1 a 2 h 2 (3)
contact point is nearly independent of the ma-
chine. It is caused by the material (effect of in the range of force immediately after force increase
microstructure such as porosity or of preparation at contact. Using Eq. (3) the extrapolation to F 5 0
such as roughness). gives the contact point, h 0 ,
3. There is no information on the actual type of
indentation function near the contact point (for
2 a1 ] a 12 a0
the use of extrapolation). The force–displacement h 0 5 ]] 1ŒR; R 5 ]2 2 ]. (4)
dependence is so different that even out of the 2a 2 4a 2 a 2
common range of constant hardness (at higher
forces in Fig. 1) linear sections can also occur (at The parameters a 0 , a 1 , a 2 including their variances
smaller forces in Fig. 3). V(a 0 ), V(a 1 ), and V(a 2 ) as well as the covariance
Cov(a 0 , a 1 ), Cov(a 0 , a 2 ), and Cov(a 1 , a 2 ) are
To take these points into account, two methods estimated by the Gauß method. The uncertainty of
can be chosen. One alternative is to leave aside all the contact point, u 2 (h 0 ), caused by the scatter of the
problems concerning the unknown, highly scattered force origin u F2 , can be calculated from the variances
indentation response near the contact point by the and covariances [10],
46 C. Ullner / Measurement 27 (2000) 43 – 51

Vsa 0d 1 u 2F Results on float glass up to 10 N are demonstrated in


2 2 2 22
u (h 0 ) 5 ]]] 2 1 H 1V(a 1 ) 1 H 2V(a 2 ) Fig. 4 (HU53600 N mm ). The contact point h 0
4a 2 R and its range of uncertainty according to Eq. (5) are
H1 H2 plotted against the upper limit of the fitting range
1 ]] ] Cov(a 0 ,a 1 ) 1 ]] ] Cov(a 0 ,a 2 ) used for the extrapolation to F 5 0. As can be seen
Œ
a2 R a 2ŒR
there is no real solution for h 0 up to about 1.2 N
1 2H1 H2 Cov(a 1 ,a 2 ) (5) (grey region). The determination of the contact point
is not possible according to Ref. [10] in this range.
1 a1 a1 a 21 2 2a 2 a 0 The experimental indentation curve fits the ideal
H1 5 ] 2 ]] ; H 5 ] 2 ]]]
2a 2 4a 22Œ]
R 2
2a 22
]
4a 32ŒR function of the depth sensing hardness,
F 5 HU ssh 2 h 0d 2 (6)
As is indicated by Eq. (4) there is no real solution of
h 0 for R , 0. Additionally, the uncertainty of h 0 after so good that regions of imaging solutions also occur
Eq. (5) increases very strongly if R approaches zero. at higher forces (near 2.5, 5, and 8 N).
This is the main point which the study focuses on. The second problem of extrapolation is the certain
The case R 5 0 occurs exactly for the ideal fitting range of the extrapolating function. The
condition of the constant hardness (homogenous contact point determined by extrapolating the func-
material, no surface effects, ideal indenter geometry). tion F(h), Eq. (3), can be strongly dependent on the
Whereas the uncertainty of the contact point in the selected fitting range. To demonstrate this, some
nanometre range is sufficiently small because the different extrapolating curves fitted in the slightly
deviations from the ideal conditions are substantial modified fitting range are plotted in Fig. 5. The
(Fig. 1 and model in Ref. [6]), the uncertainty can fitting ranges differ only by addition of the previous
become too high in the micrometre range because of data point at the lower limit of the fitting range. The
the ideal force–displacement dependence (Fig. 2). upper limit is constant. The same experimental data
have been used in Figs. 4 and 5. As can be seen from
Fig. 5 the shape of the fitting functions in the region

Fig. 4. Extrapolated contact points according to Eq. (4) after Fig. 5. Indentation data record of float glass measured by a
fitting the experimental data of float glass (tin side, R a 5 0.02 mm) hardness machine with an enhanced scatter of force before
in the range 0.05 N,F , F2 . The range of uncertainty according contact. If the fitting range, F1 , F ,1 N, is extended to the four
to Eq. (5) is shown by the two dashed lines. Note the missing real indicated data points (open squares) the shape of the curve for
solution in the four grey regions. The specifications of the extrapolating to F 5 0 becomes very different while differences of
hardness machine are given in the caption of Fig. 2. the curves within the fitting range are not visible.
C. Ullner / Measurement 27 (2000) 43 – 51 47

of extrapolation is very different whereas the func- and further materials has shown that a more detailed
tions cover within the fitting range above 1 mm well. analysis of the applied extrapolation is necessary.
The different fitting ranges result not only in differ-
ent contact points but also in cases of missing real
solutions (curves 1 and 2 in Fig. 5). 4. Analysis of extrapolation
Certainly, the test up to 10 N selected for the
demonstration of the extrapolation problems in Figs. The determination of the contact point by ex-
4 and 5 is extreme. However, fitting ranges which do trapolating the function F(h) fitted in F1 # F # F2 is
not result in real solutions of contact point h 0 after demonstrated in Fig. 7. The indentation force is
extrapolation can also exist in certain indentation normalized to the lower limit of the fitting range, F1
tests up to 1 N. Two indentation curves of the test (equals the standard deviation of the force, u F , for
plotted in Fig. 1 are selected to demonstrate the instance). Random fluctuations of the data points
indentation tests up to 1 N. Two indentation curves within the fitting range are not taken into account
of the test plotted in Fig. 1 are selected to demon- because the extrapolation problem arises from the
strate the results of h 0 after extrapolation (Fig. 6). certain shape of the extrapolation function. Instead of
The test 06 leads to a slightly variable contact point fitting within F1 # F # F2 the parameters a 0 , a 1 , a 2
if the upper limit of the fitting range is increased up of the second order polynomial, Eq. (3), are de-
to 0.1Fmax according to the standard [3]. In contrast, termined from the three data points (h 0 , 0), (h 1 , F1 ),
the test 02 does not give real solutions for the fitting (h 2 , F2 ) which give a linear inhomogenous equation
ranges among 0.00004 N,F ,0.009 N and 0.00004 system
N,F ,0.028 N. However, there are additional real
solutions of the contact point for the fitting ranges Fi 5 a 0 1 a 1 h i 1 a 2 h 2i ; i 5 0, 1, 2; F0 5 0. (7)
among 0.003 N,F ,0.028 N and 0.003 N,F ,
The zero point (0, 0) is defined by the condition
0.028 N if only the fitting range near the contact
point is reduced. F F
The practice involving further hardness machines ]21 5 ]22 . (8)
h1 h2

In this way the data points (0, 0), (h 1 , F1 ), (h 2 , F2 )


represent the ideal dependence, Eq. (6), according to

Fig. 6. Extrapolated contact points according to Eq. (4) after


fitting the experimental data of silicon nitride ceramics (syalon) in
the range F1 , F , F2 . The two curves 02 and 06 of the test in
Fig. 1 are selected. The region of missing real solutions becomes Fig. 7. The determination of the contact point by fitting the
smaller if the fitting range is started at F1 5 0.003 N instead of function F(h) in mF , F , 2mF and extrapolating to F 5 0 using
F1 5 0.00004 N. The uncertainty in force measurement is u F 5 the function F(h), Fex1 (h), or Fex2 (h) with the same slope at
0.0004 N. F 5 mF .
48 C. Ullner / Measurement 27 (2000) 43 – 51

the rule of similarity. The real indentation curve in plotted in Fig. 7. Comparing with experimental data
F1 # F # F2 can diverge from Eq. (6). In this sets demonstrated in Figs. 1–3 the shapes of the
analysis, it is defined by the given contact point (h 0 , curves in Fig. 7 make clear that there is not a
0). The contact point, h 0 , must range in 0 # h 0 # h lin favoured extrapolating function. The uncertainty due
with to the artificial extrapolating function can be esti-
mated by the difference of the calculated contact
h 1 F2 2 h 2 F1
h lin 5 ]]]]. (9) points after Eq. (12). Taking into account the
F2 2 F 1
uncertainty of the force origin, u F , the maximal
Although such a deterministic analysis cannot give contact point, h 0max , is h 01 with F1 ⇒ F1 2 u F and
the variances and covariance of the parameters a 0 , the minimal contact point, h 0min is h 02 with
a 1 , a 2 the uncertainty of the extrapolated contact F1 ⇒ F1 1 u F . The difference reads after Eq. (12)
point can be roughly estimated according to Eq. (5) F1 1 3u F
because the first term is dominant Dh 0 5 h 0max 2 h 0min 5 ]]]. (13)
a1 1 a2h1
uF
ush 0d . ]]] 5 U. (10) Finally this difference is used for normalization of
2a 2 R 0.5
the main part of the uncertainty according to Grau et
The uncertainty in force measurement is u F . We are al. [10], Eq. (10),
going to calculate the portion U of the uncertainty. U
U a1 1 a2h1
is the uncertainty for the approach of F(h) to the ]] 5 ]]]]]]]]]]]]
ideal case, Eq. (6), that means h 0 → 0 or R → 0. For
this, U is normalized to the additional uncertainty of
Dh 0 F1
]13
uF S DœS D
]
a1 2 a0
2a 2
2]
a2
the contact-point determination due to the use of the
fitting function for the extrapolation to F 5 0 instead S D F1 F2
5 f h 0, ], ] .
uF uF
(14)
of the use of a real physical function F(h). It can be
assumed that the force–depth dependence closed to Using Eqs. (7), (9), and (14) the normalized
contact, Fex (h), equals the indentation response in the uncertainty, U /Dh 0 , is plotted in Fig. 8 as a function
fitting range F1 # F # F2 . To estimate this type of of h 0 /h 0lin for three different ‘fitting ranges’ normal-
extrapolation uncertainty it is assumed that the ized to the uncertainty of the force origin, F1 /u F #
unknown force dependence Fex (h) in 0 # F # F1 is
accomplished between the two functions as follows:
on the one hand the simplest function is the linear
dependence with the same slope, A, like the fitting
function at (h 1 , F1 ). On the other hand the function is
based on the rule of similarity (ideal case). The two
functions can be written:
Fexshd 5 A msh 2 h 0md m ; m 5 1, 2 (11)
with the condition of the same slope A m 5 A of the
fitting function, Eq. (3), at F 5 F1 . The extrapolated
contact points h 01 and h 02 are
mF1
h 0m 5 h 1 2 ]]]2 ; m 5 1, 2 (12)
a 1 1 2a 2 h 1
Fig. 8. Normalized uncertainty of the contact point as a function
with h 1 as the displacement at F 5 F1 and a 1 , a 2 as
of the portion of the linear dependence of F(h) within the fitting
the limits of Eq. (3) calculated by Eq. (7). range. U /Dh 0 . 1 means the uncertainty due to the use of the
The three extrapolating functions, F(h) after Eq. second order polynomial is greater than the uncertainty of the
(3), Fex (h) after Eq. (11) with m 5 1 and m 5 2 are unknown extrapolating function.
C. Ullner / Measurement 27 (2000) 43 – 51 49

F /u F # F2 /u F . In this way the curves in Fig. 8 are • The tests with problems in extrapolation could be
independent of the uncertainty in force measurement, removed. A procedure for the selection of accept-
u F . The portion of linearity concerning the ‘fitting able tests must be found. However, the result is
function’, F(h), is given by the value h 0 /h 0lin rang- artificial regarding the stochastic materials re-
ing from h 0 /h 0lin 5 0 (ideal case according to the sponse.
rule of geometric similarity), to h 0 /h 0lin 5 1 (linear • The fitting range is varied unless the extrapolation
dependence). gives a real solution with minimal uncertainty.
However, the indefinite limits of the fitting range
can result in reduced reproducibility between
5. Discussion different machines.
• The need for determination of the contact point is
As is demonstrated by the deterministic model on avoided with the depth sensing hardness accord-
the property of contact-point extrapolation there are ing to Eq. (2). However, the current depth
three critical points of the obvious way to use a dependence of the hardness cannot be detected.
second order polynomial for both fitting and ex- • A more robust determination of contact point can
trapolating. It can be concluded from Fig. 8: be performed by the use of the inverse indentation
dependence,
1. the normalized uncertainty becomes unlimited for
the ideal case according to the rule of geometric h 5 b0 1 b1F 1 b2F 2 (15)
similarity (the procedure needs a fitting function
with a portion of linearity);
2. the normalized uncertainty drops substantially or
below one for increasing the portion of linearity
]
(the uncertainty caused by the unknown ex- h 5 b 0 1 b 1ŒF 1 b 2 F (16)
trapolating function in the contact range, Fex (h) ,
F1 , becomes dominant); with the contact point h 0 5 b 0 . The results accord-
3. the normalized uncertainty is higher if the fitting ing to the two functions are plotted in Fig. 9 using
range is closer to F 5 0 (the disadvantage of point the extreme example of Fig. 4. As shown in Fig. 9
1 cannot be weakened by a closer fitting range). the contact points for small fitting ranges below
F2 51 N are very realistic but the model error
In practice, a laboratory using one type of a increases at higher F2 related to that of the second
hardness machine can obtain results of HU with very order polynomial, F(h).
small uncertainty caused by the contact-point ex-
trapolation, if the fitting range has been optimized
regarding the certain character of data sets (sampling In every case the estimation of the uncertainty is
rate, scatter of force and displacement, portion of fundamental for the examination of the hardness
linearity). However, the uncertainty caused by the machine including the procedure of extrapolation.
unknown function, Fex (h) , F1 , near the contact Taking into account the results of the analysis it is
point can be much larger than the uncertainty caused proposed to improve the comparability as follows.
by the statistical scatter (U /Dh 0 < 1 for h 0 /h 0lin . Twice the uncertainty of the contact point is de-
0.3 in Fig. 8). For that reason, the scatter between termined from the sum of the uncertainty, Dh 0 ,
results of HU which were measured by several caused by the unknown extrapolating function,
hardness machines of different types (in different Fex (h) , F1 , and the standard deviations of the two
laboratories with different procedures for determin- types of contact points according to Eq. (12), u h 01 or
ing the contact point) can become much higher than m 5 1, and u h 02 for m 5 2,
the scatter of results within one laboratory.
There are several ways to avoid the critical points Dh 0 1 u h 01 1 u h 02
which have been indicated by the analysis. Uh 0 5 ]]]]] (17)
2
50 C. Ullner / Measurement 27 (2000) 43 – 51

every fitting range. The high fluctuations below 1 N


in Fig. 9 are caused by the certain extreme example
of the used data record which is not optimal near the
contact point.

6. Conclusion

The use of the depth sensing hardness HU accord-


ing to Eq. (1) makes it necessary to determine the
contact point. Analysing the procedure for determin-
ing the contact point (problems of fitting and ex-
trapolating) a polynomial of second order is appro-
priate for use only in selected cases of the test
reality. There are no real solutions or results with
Fig. 9. Additional to the contact points (full rhombs) and their enhanced uncertainty for specified fitting ranges of
uncertainties (dashed line) in Fig. 4 the contact points h 01 (2) and some tests. The uncertainty contribution of the type
h 02 (1) according to Eq. (12) as well as the uncertainties of the extrapolation function should be involved. For
according to Eq. (15) after fitting the experimental data in the the estimation of the current uncertainty of the
range 0.05 N,F , F2 are plotted (solid line). Note there are real
contact point it is advantageous to use the contact-
solutions for every fitting range. The contact points extrapolated to
Eq. (17) (hole spheres) and Eq. (18) (hole triangle) could be used point procedure according to Eq. (17) and (18)
for the simplification. because a real solution is obtained in every case and
the uncertainty of the unknown extrapolating func-
tion is taken into account. For simplification of the
u 2(h 0m ) 5 H 02 (V(a 0 ) 1 u F2 ) 1 H 21 V(a 1 ) 1 H 22 V(a 2 ) contact-point procedure, it is recommended that the
inverse dependence according to Eq. (15) is used.
1 2H0 H1 Cov(a 0 ,a 1 ) 1 2H0 H2 Cov(a 0 ,a 2 )
The estimation of the uncertainty involving the
1 2H1 H2 Cov(a 1 ,a 2 ) m 5 1,2 (18) contribution of extrapolation according to Eqs. (17)
and (18) is important to the reliability inspection of
mF1 1 the hardness machine.
H0 5 ]]]2Œ]
1 ]] ];
4a 2 R
3
2a 2ŒR
mF1 a 1 1 a1
H1 5 ]]] ] 2 ] 1 ]] ; Acknowledgements
8a 2ŒR
3 3 2a 2 4a 22Œ]
R
The author gratefully acknowledges the ‘Deutsche
mF1 a 12 mF1 (F1 2 a 0 ) (1 2 m)F1 Forschungsgemeinschaft’ for the financial support of
H2 5 ]]]4Œ]
1 ]]]] 3 ]
1 ]]] ]
4a 2ŒR 2a 22ŒR the project ‘Depth sensing hardness on ceramics’.
3 3
8a 2 R
2
a1 a 1 2 2a 2 a 0
2 ]2 2 ]]] ] .
2a 2 4a 32ŒR References

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Fig. 9. It can be seen that the upper limit of Engineering), Springer, Berlin, 1898, p. 234.
[2] W. Weiler, Hardness testing — a new method for economical
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according to Eq. (17), (18) yields real solutions for October, 1997.
C. Ullner / Measurement 27 (2000) 43 – 51 51

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