SIMULTANEOUS MEASUREMENT OF GRAIN SIZE AND SHAPE FROM ULTRASONIC BACKSCATTERING MEASUREMENTS MADE FROM A SINGLE SURFACE Y. Guo, R. B. Thompson, and F. J. Margetan Center for Nondestructive Evaluation Iowa State University Ames, Iowa 50011, USA ABSTRACT. Ultrasonic techniques for the characterization of grain size have been investigated for over two decades, including important practical applications. Generally, however, these make the assumptions that the grains are equi-axed. In this paper, we consider the more general case in which the grains are elongated. Inversion procedures are presented to infer the geometrical parameters of the grains from various combinations of attenuation and backscattering data. To provide a theoretical foundation, an expression is presented relating the ultrasonic backscattering coefficient to the geometrical parameters of the grains for shear incidence waves and its experimental verification is reported. This complements previously reported theories for backscattering and attenuation of longitudinal waves. Measurement results are presented which demonstrate the effectiveness of these new sizing approaches on a set of aluminum samples that were rolled as either rods or plates. One of the techniques has the major practical advantage that all data (backscattering) can be taken from the single side of a sample with no requirements for a parallel back surface. INTRODUCTION The characterization of the microstructure of materials is an important NDE application, with a primary motivation being the control of mechanical properties. Ultrasonic measurements have a long history of application in this area based on the dependence of both attenuation and backscattering on grain size [1-3]. Early approaches were based on a direct measurement of attenuation, an application restricted to parts with parallel surfaces [1,2]. The desire for a technique for single sided measurements on parts of complex geometry led to a backscattering approach [3]. However, the objective remained to infer grain size from attenuation, with the latter being inferred from the rate of decay of the backscattered noise. Most recently, Good has used the time dependence of the backscattered noise to gain information about microstructural changes, for example those associated with hardening processes [4]. All of these techniques have produced valuable results in appropriate application areas. However, to the knowledge of the authors, the primary applications have been to microstructures in which the grains are equi-axed. It can be speculated that this is a direct CP657, Review of Quantitative Nondestructive Evaluation Vol. 22, ed. by D. O. Thompson and D. E. Chimenti © 2003 American Institute of Physics 0-7354-0117-9/03/$20.00 1347 consequence of the fact that only a single parameter is inferred from the measurements, e.g. the attenuation. Obviously, one parameter can only provide information about a single attribute of the microstructure, e.g. grain size. In this work, we seek new techniques that can provide information on both grain size and shape. The motivation for our approach was a series of measurements reported in a previous volume of this series [5]. Measurements of attenuation and backscattering were reported on a set of aluminum samples with elongated grains produced by rod and plate rolling. It was observed that, whereas the backscattering was highly anisotropic as expected, the attenuation varied only slightly with direction. In the concluding remarks, it was suggested that a better understanding of these effects could lead to improved techniques for microstructural characterization. Further discussion of the initial observations has been provided by Thompson [6]. In this paper, we will describe three methods that were examined with the objective of the simultaneous determination of" grain size and shape. The initial motivation was to take advantage of this fundamental difference in the dependence of attenuation and backscattering on grain parameters. After a brief review of the sample characteristics, the three methods will be described. The first two were motivated by gaining an increased understanding of the underlying measurement principles and impose restrictions on the sample geometry. The final technique utilized only data that could be obtained from one surface without the availability of a second, parallel surface. SAMPLES The aluminum alloy samples, including micrographs, have been previously described [5,6]. Table 1 lists the average grain dimensions, as inferred from an analysis of micrographs. Two samples had "cigar-shaped" grains, with an elongation of more that 10:1. The other two had "pancake-shaped" grains, also with an aspect ratio of more that 10:1. In both cases, the defects were ellipsoidal rather than spheroidal, i.e. there was no axis of rotational symmetry. THEORY A theoretical description of the effects of grain elongation on attenuation and backscattering is a key element of our approaches. Description of those theories is beyond the scope of this paper. The starting points are theories initially reported by Stanke and Kino for attenuation [7] and Rose for backscattering [8] for equi-axed grains . Extensions to elongated grains and other complex microstructures include contributions by Ahmed, Han and Panetta, and references to those works may be found in [6]. The predictions of those theories have been found to be in semi-quantitative agreement with the previously reported measurements on the aluminum samples that are the subject of this study [5]. TABLE 1. Average grain dimensions (semi-axes) in microns. Sample Tl T2 T3 T4 2-axis (b) 45 17 60 65 1-axis (a) 52 35 170 183 1348 3-axis (c) 539 420 17 12 METHOD A: SIMULTANEOUS MEASUREMENT OF ATTENUATION AND BACKSCATTERING METHOD A: SIMULTANEOUS MEASUREMENT OF ATTENUATION AND BACKSCATTERING The basic idea in Method A is to measure both the attenuation and the absolute level ofThe thebasic backscattering, as Aquantified by aboth material propertyand known as the idea in Method is to measure the attenuation the absolute backscattering for waves propagating single direction, normal level of the coefficient, backscattering, as quantified by in a amaterial property i.e., known as to thea part surface. Grain size parameters attenuation backscattering models are to then backscattering coefficient, for waves in propagating in and a single direction, i.e., normal a adjusted to optimize experiment theory. In models our employment part surface. Grain the sizeagreement parametersbetween in attenuation and and backscattering are then ofadjusted the technique, we have assumed that a sample is available with two parallel surfaces. to optimize the agreement between experiment and theory. In our employment However, we note that the same information could be obtained with single-sided access if of the technique, we have assumed that a sample is available with two parallel surfaces. the attenuation werethat inferred frominformation the rate of decay of the backscattered noise [3].access if However, we note the same could be obtained with single-sided Figure 1were illustrates basic this plot, grains werenoise assumed the attenuation inferredthefrom theidea. rate ofIndecay of thethe backscattered [3]. to have two of the three1 major axesthe (a,b,c) Thethis wave to propagate in have the b Figure illustrates basicequal. idea. In plot,was the assumed grains were assumed to direction andthree it was assumed that a =equal. b for The samples andassumed T2, andtob propagate = c for samples two of the major axes (a,b,c) waveT1was in the T3 b and T4. The ratio (b/c fora = T1b and T2, b/a Tl forand T3 T2, andand T4)b would small T3 for direction and itaspect was assumed that for samples = c for be samples samples andaspect T2 and forTlsamples PartT4) (a)would showsbea small plot offora and T4. T1The ratiolarger (b/c for and T2,T3b/aand forT4. T3 and theoretical of attenuation, at a frequency as shows a function of of grain samples Tlprediction and T2 and larger for samples T3 and of T4.7 MHz, Part (a) a plot a volume andprediction aspect ratio. It is interesting to note of that, for theas range of parameters theoretical of attenuation, at a frequency 7 MHz, a function of grain volume and ratio.is much It is interesting to note that, volume for thethan range of shape. parameters examined, the aspect attenuation more sensitive to grain grain Part examined, the attenuation much grain volume than grain shape. Part (b) shows the comparableisplot formore the sensitive predictedtobackscattering coefficient, a material (b) shows comparable plot for of thethe predicted backscattering coefficient, a material property thatthe quantifies the capacity microstructure to generate noise. Techniques quantifies thecoefficient capacity of microstructure to generate noise. Techniques toproperty infer thethat backscattering or the its square root (FOM) from experimental data are to infer the backscattering or its root from experimental data are discussed elsewhere [9]. Itcoefficient is interesting to square note that the(FOM) dependence of the backscattering discussed [9]. It isparameters interesting to the dependence thethe backscattering on the twoelsewhere microstructural is note quitethat different than thatofof attenuation, on the twowith microstructural parameters different data. than that of suggests the attenuation, consistent the previously reportedis quite experimental This that a consistent with the previously reported experimental data. suggests a measurement of attenuation and backscattering on the same sampleThis would providethat a way of determine attenuationgrain and backscattering on the samePart sample would provide tomeasurement independently volume and aspect ratio. (c) illustrates this inaaway plot to independently grain volume ratio. value Part (c) this in a plot of grain volume determine versus aspect ratio. and Foraspect a given of illustrates either attenuation or of grain volume versus aspect ratio. For a given value of either attenuation or backscattering alone, there is a family of {volume, aspect ratio} pairs, lying on a curved backscattering alone, there is aforfamily of {volume, aspect ratio} pairs, lying on a curvedif line, that could be responsible that value of attenuation or backscattering. However, line, that could be responsible for that value of attenuation or backscattering. However, if attenuation and backscattering have both been measured, the grain volume and aspect attenuation and backscattering have both been measured, the grain volume and aspect ratio are uniquely defined by the intersection of these lines. It is interesting to note, that ratiothearecase uniquely definedthebytwo the intersection theseorthogonal, lines. It is indicating interesting that to note, for illustrated, curves are of nearly the that two for the case illustrated, the two on curves are nearlyoforthogonal, measurements have good leverage the quantities interest. indicating that the two measurements have good leverage on the quantities of interest. K10 6 Volume (Micron**3) FIGURE FIGURE1.1.(continued) (continued) Volume (Micron**3) (a) (a) (b) (b) 1349 6 x 10 5 6 x 10 5 4.5 fixed backscattering fixedbackscattering attenuation fixed fixed attenuation 4.5 4 r 4 3.5 ) 3.5 3 3 )** n 3*o 3 *r nci 2.5 orM ci ( 2.5 e M (m 2 eul 2 mo ulV 1.5 o V 1.5 1 1 0.5 0.5 0 0 0 0 0.2 0.2 0.4 0.4 0.6 0.6 0.8 1 1.2 0.8 Aspect 1 ratio 1.2 Aspect ratio 1.4 1.4 1.6 1.6 1.8 1.8 2 2 (c) (c) FIGURE 1. Determination of grain size and shape from attenuation and backscattering data. (a) FIGURE 1. 1. Determination Determination of of grain grain size size and and shape shape from attenuation attenuation and andbackscattering backscatteringdata. data, (a) (a) Attenuation versus grain volume and aspect ratio atfrom 7 MHz. (b) Backscattering versus grain volume and Attenuation versus grain grain volume volume and and aspect ratio ratio atat 77 MHz. MHz. (b) (b) Backscatteringversus versusgrain grainvolume volumeand and aspect ratio at 7 MHz. (c) Illustrationaspect of determination of grain Backscattering volume and aspect ratio from knowledge of aspect ratio at 7 MHz. MHz. (c) (c) Illustration Illustration of ofdetermination determinationof ofgrain grainvolume volumeand andaspect aspect-1ratio ratiofrom fromknowledge knowledge ofof 3 attenuation and backcscattering. (Units: Attenuation, Np/cm, backscattering, cm-11 , volume, µm3 3.) attenuation and backcscattering. backcscattering. ((Units: Attenuation, Np/cm, Np/cm, backscattering, backscattering,cm cm' ,,volume, volume,µm Jim.).) Units: Attenuation, 300 300 600 600 Micrograph Micrograph 500 Ultrasound §500 500 Ultrasound 400 | 400 400 300 0^300 300 H N 200 ^200 200 100 T2 '£ 100 100 T2 0 0 0o 1-axis 2-axis 3-axis 400 2-axis 3-axis 400 n 1-axis _400 Micrograph Direction T4 C/5 Micrograph Micrograph Direction T4 Ultrasound 300 Ultrasound Ultrasound 300 §300 Grain GrainSize Size(microns) (microns) 600 600 500 500 400 400 300 300 200 200 100 100 0 0 400 400 Micrograph Micrograph Ultrasound Ultrasound T1 T1 1-axis 1-axis 2-axis 2-axis Micrograph Direction Micrograph Direction Ultrasound Ultrasound 3-axis 3-axis T3 T3 Grain GrainSize Size(microns) (microns) Grain GrainSize Size(microns) (microns) Grain GrainSize Size(microns) (microns) Figure 2 presents results of an experimental test of this idea. The previously Figure 2 presents presents results results of of an an experimental experimental test test of of this this idea. idea. The The previously previously measured values of the attenuation and backscattering served as inputs and the data was measured values of of the the attenuation attenuation and and backscattering backscattering served served as as inputs inputs and and the the data datawas was interpreted using the procedures illustrated in Figure 1. In this comparison, it had to be interpreted using the the procedures procedures illustrated illustrated in in Figure Figure 1.1. In In this this comparison, comparison, itithad hadtotobe be assumed that a = b for the grains. There is good overall agreement between the predicted for the grains. grains. There There is is good good overall overall agreement agreement between between the the predicted predicted assumed that aa == bb for and observed values of the grain size parameters. of the the grain grain size size parameters. parameters. and observed values of 200 200 N C/) 100 100 0 0 200 200 100 .£ 100 100 05 5 1-axis 1-axis 1-axis 2-axis 3-axis 2-axis 3-axis 2-axis 3-axis Direction Direction Direction 0 0o 1-axis 1-axis 1 -axis 2-axis 3-axis 2-axis 2-axis 3-axis 3-axis Direction Direction Direction FIGURE 2. Comparison of ultrasonically predicted and actual grain sizes for all samples based on Method FIGURE 2. FIGURE 2. Comparison Comparisonof ofultrasonically ultrasonicallypredicted predictedand andactual actualgrain grainsizes sizesfor forall allsamples samplesbased basedon onMethod Method A. A. A. 1350 L-wave .rwave L-wave L-wave T-wave T-wave T wave ' 1-axis 1-axis 1-axis '* !-axis 3-axis L-wave L-wave 2-axis 3-axis 2-axis L-wave L-wave FIGURE 3. Schematic illustration of Methods B (left) and C (right) based on backscattering measurements FIGURE 3. Schematic illustration of Methods B (left) and C (right) based on backscattering measurements alone. alone. METHOD B: MEASUREMENT OF BACKSCATTERING FOR WAVES METHOD B: MEASUREMENT OF BACKSCATTERING FOR WAVES PROPAGATING IN THREE ORTHOGONAL DIRECTIONS PROPAGATING IN THREE ORTHOGONAL DIRECTIONS Since the backscattering is more sensitive to the grain aspect ratio than is the Since the backscattering is more sensitive to the grain aspect ratio than is the attenuation, and since backscattering measurements do not require parallel surfaces, the attenuation, and since backscattering measurements do not require parallel surfaces, the possibility of recovering grain grain size size and andshape shapefrom frombackscattering backscatteringmeasurements measurementsalone alone possibility of recovering was examined. Figure 3 illustrates both Method B and Method C. In the former, was examined. Figure 3 illustrates both Method B and Method C. In the former, thethe longitudinal wave wave backscattering backscattering isis measured measured for for waves wavespropagating propagatingalong alongthree three longitudinal orthogonal directions. Although this is generally not possible in the laboratory, it provides orthogonal directions. Although this is generally not possible in the laboratory, it provides means of of examining examining the the leverage leveragethat thatbackscattering backscatteringhas hasononthethegrain grainsize sizeand andshape. shape. aa means For future future reference, reference, the the configuration configuration used used inin Method Method CCis isalso alsoshown. shown. The The For backscattering is is measured measured for forlongitudinal longitudinalwaves wavesatatnormal normalincidence incidenceand and transverse backscattering forfor transverse waves at at oblique oblique incidence incidencein intwo twoorthogonal orthogonalplanes. planes. waves To test Method B, an algorithm was written whichdata datapropagating propagating three To test Method B, an algorithm was written ininwhich in in thethe three orthogonal directions was compared to the theoretical predictions of the backscattering orthogonal directions was compared to the theoretical predictions of the backscattering models [6,8]. [6,8]. The The degree degree of of agreement agreementininaaleast leastsquares squaressense sensewas wascomputed computedand and models thethe values of of the the grain grain size size and and shape, shape, (a,b,c), (a,b,c),were werevaried variedtotoobtain obtainbest bestfit.fit.Figure Figure4 4shows shows values the results. results. Although Although there there appear appear totobebesome somesystematic systematicdisagreements disagreementsforforthethelarger larger the dimensions, there there isis generally generallygood goodagreement. agreement. dimensions, METHOD C: C: SINGLE-SIDED SINGLE-SIDEDMEASUREMENT MEASUREMENTOF OFBACKSCATTERING BACKSCATTERING FOR METHOD FOR NORMAL LONGITUDINAL LONGITUDINALAND ANDOBLIQUE OBLIQUESHEAR SHEARWAVES WAVES The ofof Figure 3. 3.ToTo The basic basic strategy strategyof ofMethod MethodCCisissketched sketchedininthe theright righthand handside side Figure test this, a theory was developed, theory for for the thebackscattering backscatteringcoefficient coefficientfor fortransverse transversewaves waves was developed, with the result result (for (for cubic cubic crystallites crystalliteswith withrandomly randomlyoriented orientedprincipal principalaxes) axes) η (ω ) = 3k 4 ( C11 − C12 − 2C 44 ) ( 175 4πρ v 2 t ) 2 1351 2 v ò P (s) e v 2 ikˆe⋅ s v d 3s (1) 400 300 200 T1 100 0 1-axis Grain Size (microns) Grain Size (microns) 500 Micrograph Ultrasound 400 300 2-axis Direction Micrograph Ultrasound 3-axis Grain Size (microns) Grain Size (microns) 600 600 i T3 200 100 0 11-axis -axis 2-axis 3-axis 3-axis 2-axis Direction Direction 600 500 Micrograph Ultrasound 400 300 200 T2 100 0 1-axis 2-axis 3-axis 1 -axis 2-axis 3-axis Direction 400 Micrograph T4 Ultrasound 300 200 100 0 1-axis 1 -axis 2-axis 3-axis 3-axis 2-axis Direction Direction FIGURE 4. 4. Comparison Comparisonofofultrasonically ultrasonicallypredicted predictedand andactual actual grain sizes samples based Method grain sizes forfor samples based on on Method B. B. FIGURE where pρ is is the the density, density,vvisisthe thetransverse transversewavespeed, wavespeed,C/yCare crystallite elastic constants, where crystallite elastic constants, k k IJ are v theprobability probabilitythat thattwo tworandomly randomly selected points, separated is the the wavevector, wavevector, and andP(s) P( s )isisthe is selected points, separated v by a vector s , lie in the same grain. It is interesting to note that, for a given material andand by vector s , lie in the same grain. It is interesting to note that, for a given material frequency, larger than thatthat forfor frequency, the the predicted predictedtransverse transversewave wavebackscattering backscatteringis issignificantly significantly larger than longitudinal is is shorter forfor transverse longitudinal waves. waves. This Thisisisaaresult resultofoftwo twoeffects, effects,thethewavelength wavelength shorter transverse waves which is the physical waves and and hence hence closer closer totothe thegrain grainsize, size,and andthe theelastic elasticanisotropy, anisotropy, which is the physical cause for forfor longitudinal waves. for the the backscattering, backscattering,isisgreater greaterfor forshear shearwaves wavesthan than longitudinal waves. Figure Figure 55 shows shows aa test test ofof this this theory theory against againstnew newmeasurements measurementsof ofthethe backscattering for transverse waves propagating at 45 degrees with respect to to thethe sample backscattering for transverse waves propagating at 45 degrees with respect sample normal. The 4-axis and 5-axis correspond, respectively, to propagation in the 1-2 plane normal. The 4-axis and 5-axis correspond, respectively, to propagation in the 1-2 plane and the were input to to and the 2-3 2-3 plane plane respectively respectively(see (seeFig. Fig.3). 3). Measured Measuredgrain grainsize sizeparameters parameters were input the model, and reasonably good agreement with experiment is observed with no adjustable the model, and reasonably good agreement with experiment is observed with no adjustable model parameters. model parameters. As thethe backscattering As was was done done for for Method MethodB,B,ananalgorithm algorithmwas waswritten writtenininwhich which backscattering data for longitudinal and transverse waves propagating in the various directions data for longitudinal and transverse waves propagating in the various directionswaswas compared to the theoretical predictions of the backscattering models. The degree of compared to the theoretical predictions of the backscattering models. The degree of agreement in a least squares sense was computed and the values of the grain size and agreement in a least squares sense was computed and the values of the grain size and shape, (a,b,c), were varied to obtain a best fit. Figure 6 shows the results, which are very shape, (a,b,c), were varied to obtain a best fit. Figure 6 shows the results, which are very similar to those obtained with Method B. Although there appear to be some systematic similar to thoseforobtained with Method B. Although theregood appear to be some disagreements the larger dimensions, there is generally agreement. Thissystematic is very disagreements for the larger dimensions, there is generally good agreement. very encouraging since this data was obtained in a single-sided measurement and This doesisnot encouraging since this data was obtained in a single-sided measurement and does require a second, parallel surface. We note that for all three techniques we assumed thenot require a second, of parallel surface. We that forthat all crystalline three techniques we assumed elastic constants pure aluminum, andnote assumed axes were randomlythe elastic constants of pure aluminum, and assumed that crystalline axes were randomly oriented. oriented. 1352 0.25 0.20 0.15 Exp (4-axis) The (4-axis) Exp (5-axis) The (5-axis) 0.10 0.05 0.00 0 0.30 ,0.30 Figure of Merit (cm**-0.5) Figure of Merit (cm**-0.5) T1 5 10 15 10 15 Frequency Frequency (MHz) (MHz) Exp (5-axis) The (5-axis) Exp 4-axis) The (4-axis) 0.25 0.20 T3 0.15 0.10 0.05 0.00 0.00 00 55 10 15 10 15 Frequency Frequency (MHz) (MHz) 0.30T 0.30 0.25 0.20 0.10 T2 0.05 0.00 0 20 20 Exp (4-axis) The (4-axis) Exp (5-axis) The (5-axis) 0.15 20 20 Figure of Merit (cm**-0.5) Figure of Merit (cm**-0.5) 0.30 ,0.30 0.30 0.30 5 10 15 5 10 15 Frequency ( (MHz) Frequency MHz) Exp (5-axis) The (5-axis) Exp (4-axis) The (4-axis) 0.25 0.20 20 20 T4 0.15 0.10 0.05 0.00 00 55 10 15 10 15 Frequency (MHz) (MHz) Frequency 20 20 FIGURE to experiment. experiment. FIGURE 5. 5. Comparison Comparison of of the the theory theory for for transverse transverse wave wave backscattering backscattering to CONCLUSIONS CONCLUSIONS Three determining grain grain size size and and shape shape were were Three methods methods for for simultaneously simultaneously determining evaluated based on on rolled rolled rod rod and and plate plate of of an an aluminum aluminum alloy. alloy. Each Each evaluated based on measurements measurements on measurement to produce produce good good results. results. Method Method A A requires requires both both measurement scheme scheme was was shown shown to attenuation waves propagating propagating in in the the same same direction. direction. attenuation and and backscattering backscattering information information for for waves Although with parallel parallel surfaces, surfaces, this this could could be be Although our our measurements measurements were were made made in in samples samples with implemented were inferred inferred from from the the rate rate of of decay implemented from from aa single single surface surface if if the the attenuation attenuation were decay of of the the backscattering. backscattering. Method practical application, application, but but as as aa test test of of the the leverage leverage Method B B was was not not intended intended for for practical of the needed needed size size and and shape shape of backscattering backscattering data data at at multiple multiple angles angles in in gathering gathering the information. information. The The positive positive results results led led to to the the evaluation evaluation of of Method Method C, C, which which has has the the desired desired attributes for aa second, second, parallel parallel attributes of of aa single single sided sided measurement measurement without without the the requirement requirement for surface. surface. These be imagined, These measurements, measurements, and and variants variants that that could could be imagined, show show great great promise promise of of extracting than is is commonly extracting more more information information about about grain grain size size and and shape shape than commonly done. done. A A key key ingredient ingredient is is aa theoretical theoretical basis basis to to interpret interpret multiple multiple measurements, measurements, in in one one sense sense aa form form of of data data fusion. fusion. ACKNOWLEDGEMENTS ACKNOWLEDGEMENTS This Cooperative Research This work work was was supported supported by by the the NSF NSF Industrial/University Industrial/University Cooperative Research Program Program in in Nondestructive Nondestructive Evaluation. Evaluation. 1353 600 500 §500 - 400 -| 400 300 300 0 300 200 200 <^ 200 100 100 £ 100 0 0 N 0 1-axis Grain Size (microns) T1 400 2-axis Direction Micrograph Ultrasound 300 3-axis 400 400 T3 Micrograph -^-Micrograph Ultrasound ~*~~ Ultrasound 300\ 300 | T2 T2 / / s~ *^^//^ 11-axis -axis Grain Size (microns) Grain Size (microns) Micrograph Ultrasound Grain Size (microns) 600 'c/T 500 §500 400 _600 i I 2-axis 3-axis 3-axis 2-axis Direction Micrograph Ultrasound T4 T4 E, 200 0)200 200 .N CO 100 100.E 100 0 11-axis -axis 2-axis 3-axis 2-axis 3-axis Direction Direction 0 11-axis -axis 2-axis 3-axis 3-axis 2-axis Direction Direction FIGURE6.6. Comparison Comparisonofofultrasonically ultrasonicallypredicted predictedand andactual actualgrain grainsizes sizesfor forsamples samplesbased basedononMethod MethodC.C. FIGURE REFERENCES REFERENCES 1.1. 2.2. 3. 3. 4.4. 5.5. 6. 6. 7.7. 8. 8. 9. 9. 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