`
`OF
`
`BOBBY BENNBTI
`
`STBVE TREADWAY
`
`AND
`
`DEREK HEA 1ll
`
`FOR
`
`FOR
`
`ENDODONTIC INSTRUMENT Wrm MODIFIED MEMORY AND FLEXIBILITY PROPERTIES AND
`MEnloo
`
`Bobby Bennett
`8 Sheffield Court
`Johnson City Tennessee, 37604
`Citizen of the United States of America
`
`Steve Treadway
`639 Old Embreeville Rd.
`Jonesborough Tennessee, 37659
`Citizen of the United States of America
`
`Derek Heath
`IS 16 Ocean Drive
`Vero Beach Florida, 32967
`Citizen of the United States of America
`
`LUEDBKA, NEELY & GRAHAM
`P.O. Box 1871, Knoxville 1N 37901
`
`1.865.546.4305
`1.865.523.4478
`
`(Tel)
`(Fax)
`
`MGraham@LNO-Patent.com
`
`Attorney Docket:
`
`65468.PV
`
`GOLD STANDARD EXHIBIT 2031
`US ENDODONTICS v. GOLD STANDARD
`CASE PGR2015-00019
`
`
`
`Attorney Docket No. 65468.PV
`
`BACKGROUND
`
`[0001] The present invention relates to endodontic instruments and to methods of making such
`In particular, the invention relates to nickel-titanium or ''NiTi" endodontic
`instruments.
`instruments that exhibit beneficial properties and characteristics for working in a manner so as to
`avoid difficulties associated with prior instruments including, but not limited tos undesired lateral
`transportation in curved canals, difficulties with enlarging curvilinear canals while substantially
`maintaining the original center axis of the canals, and problems with binding and/or "screwing
`in" of prior NiTi instruments in such canals.
`
`BRIBJ.I' DESCRIPTION OF THE DRAWINGS
`
`(0002] Further features, aspects, and advantages of the present disclosure will become better
`understood by reference to the following detailed description, appended claims, and
`accompanying figures, wherein elements are not to scale so as to more clearly show the details,
`wherein like reference nwnbers indicate like elements throughout the several views, and
`wherein:
`
`[0003] FIG. lA shows a further somewhat schematic representation of a tooth root canal being
`operated on using a dental instrument;
`
`[0004] FIG. 1 B shows a somewhat schematic representation of a tooth being operated on using a
`dental instrument;
`
`[0005] FIG. 2 shows a two-dimensional plot of torque data (vertical axis) versus angular
`deflection data (horizontal axis) for untreated ("control") NiTi instruments;
`
`[0006] FIG. 3 shows a two-dimensional plot of the data in FIG. 2 wherein the data sets have
`been fitted to conform to third degree polynomial equation curves;
`
`(0007] FIG. 4 shows a two-dimensional plot of torque data (vertical axis) versus angular
`deflection data (horizontal axis) for several NiTi instruments treated according to one
`embodiment of the invention;
`
`Page2of13
`
`
`
`Attorney Docket No. 65468.PV
`
`(0008) FIG. 5 shows a two-dimensional plot of torque data (vertical axis) versus angular
`deflection data (horizontal axis) for several NiTi instruments treated according to another
`embodiment of the invention;
`
`(0009] FIG. 6 shows a two-dimensional plot of torque data (vertical axis) versus angular
`deflection data (horizontal axis) for several NiTi instruments treated according to a further
`embodiment of the invention;
`
`(0010] FIG. 7 shows a two-dimensional plot of torque data (vertical axis) versus angular
`deflection data (horizontal axis) for several NiTi instruments treated according to an additional
`embodiment of the invention;
`
`(0011] FIG. 8 shows a two-dimensional plot of the data in FIG. 7 wherein the data sets have
`been fitted to conform to third degree polynomial equation curves;
`
`[0012] FIG. 9 shows an apparatus used to test cyclical fatigue of a dental instrument;
`
`[0013] FIG. 10 shows a two-dimensional plot of torque data (vertical axis) versus angular
`deflection data (horizontal axis) for twenty NiTi instruments treated according to an embodiment
`of the invention;
`
`(0014] FIG. 11 shows a two-dimensional plot of the data in FIG. 10 wherein the data sets have
`been fitted to conform to third degree polynomial equation curves; and
`
`[0015] FIG. 12 shows the two-dimensional plot of torque data (vertical axis) versus angular
`deflection data (horizontal axis) shown in FIG. 11 further including a superimposed curve
`generated from the average values of the coefficients for the third degree polynomial equations
`used to fit the data from FIG. 10 in the curves shown in FIG. 11.
`
`Page 3 of13
`
`
`
`Attorney Docket No. 6S468.PV
`
`DET~EDD~ON
`
`[0016] Various terms used herein are intended to have puticular meanings. Some of these terms
`are defined below for the purpose of clarity. The definitions given below are meant to cover all
`forms of the words being defined (e.g., singular, plural, present tense, past tense).
`If the
`definition of any term below diverges from the commonly understood and/or dictionary
`definition of such term, the definitions below control.
`
`mN: the force unit symbol for milli-Newton.
`
`m: the length unit symbol for meter.
`
`mm: the length unit symbol for millimeter.
`
`Working portion: That part of an endodontic instrument which includes surface features for
`removing material from a root canal including, but not limited to, surface features for scraping,
`shaving, cutting, penetrating, excavating, and/or removing material from canal wall surfaces in
`an effort to shape and/or enlarge a root canal.
`
`[0017) FIGS. lA and 18 show somewhat schematic representations of a tooth 10 including a
`natural root canal 12 in which an endodontic instrument 14 is being used to extirpate the natural
`root canall2. When devices such as the endodontic instrument 14 shown in FIG. lA are made
`from nickel-titanium (or ''NiTI" or ''Nitinol''), such devices tend to have improved flexibility
`properties relative to similar devices made of stainless steel. This property of NiTi and other
`similar alloys is sometimes referred to in part as superelasticity or psuedoelasticity and is often
`lauded as a unique and beneficial characteristic of endodontic tiles made from NiTi.
`
`[0018] A3 FIG. lA shows, however, when NiTi endodontic devices such as tapered files are
`used to navigate, for example, the natural root canal 12 of the tooth 10, the tendency of the
`device 14 to veer to a path contrary to the natural root canal 12 shape is a continuous concern for
`a dental practitioner-particularly when the instrument is used along a natural root canal with
`excessive curvature. A first deviation path 16 and a second deviation path 18 are shown in FIG.
`lA to illustrate the manner in which an instrument made ofNiTi tends to create disproportionate
`lateral forces along an inner surface 20 of the natural root canall2 at certain locations. If this
`
`Page4of13
`
`
`
`Attorney Docket No. 6S468.PV
`
`tendency is not carefully monitored by a dental practitioner, such instrument could easily (and
`often does) deviate from the natural root canal 12, boring an artificial structure which has the
`potential to compromise an entire tooth structure.
`
`[0019] In an attempt to address the drawbacks associated with NiTi dental instruments as used in
`endodontic procedures discussed above, the inventor bas performed a number of experiments in
`an effort to increase the beneficial flexibility properties of NiTi which, in tum, decreases the
`lateral forces exerted by a NiTi dental instrument on the inner surface of a tooth root canal. The
`inventor has surprisingly found a method for treating machined NiTi instruments that increases
`the flexibility of such instruments.
`
`(0020] In a first study, the Applicant performed twenty five tests using ADA guidelines
`(discussed infra) on five groups of endodontic files for properties including torque and angular
`deflection to see if various beat treatment methods had any effect on the relative performance of
`the files. Trends of interest became apparent based on the visual "signature" of each set of data
`sets. Table 1 below indicates relationships between each group of tests with various parameters.
`
`TABLEt
`
`Ave. Torque
`(mN·m)
`about2
`less than 2
`unstable data
`unstable data
`about2
`
`Ave. Ansular Deflection
`(Revolutions)
`1.61
`2.89
`3.32
`3.69
`4.05
`
`Control Group
`Experimental Group 1
`Experimental Group 2
`Experimental Group 3
`Experimental Group 4
`
`[0021] Graphs shown in FIGS. 2-8 plot torque (vertical axis) versus angular deflection
`(horizontal axis). In each of the graphs shown in FIGS. 2-8, 240 measurement samples for
`torque versus angular deflection were taken per one full axial (twisting) revolution of the
`instrument. FIG. 2 shows a graph of four data sets representing four separate test samples
`included in the control group which included only NiTi instruments that had not been heat
`treated according to Applicant's treatment method. A fifth data set in the control group was
`discarded because of a testing fault with the sample. As can be seen in FIG. 2, all ofthe test runs
`of the control group displayed a similar graphical signature which is more easily seen in FIG. 3
`
`PageS of13
`
`
`
`Attorney Docket No. 6S468.PV
`
`wherein the data associated with each test sample was used to generate a second order
`polynomial trend line.
`
`[DOll) Each of FIGS. 4~8 show data sets of wire samples that have been heat treated by being
`placed in a stainless steel pan and inserted into an oven which was pre~heated to about 500 °C.
`The difference between the experimental groups was the amount of time the test samples of a
`particular group were kept in the oven. FIG. 4, for example, shows a graph of five data sets
`representing five separate test samples included in the first experimental group which remained
`in the oven for 15 minutes. FIG. 5 shows a graph of five data sets representing five separate test
`samples included in the second experimental group which remained in the oven for 45 minutes.
`FIG. 6 shows a graph of five data sets representing five separate test samples included in the
`third experimental group which remained in the oven for 90 minutes. FIG. 7 shows a graph of
`five data sets representing five separate test samples included in the fourth experimental group
`which remained in the oven for 120 minutes. FIG. 8 shows second order polynomial trend lines
`based on the data sets of the fourth experimental group so that the respective "signatures" of
`these data sets can be more clearly seen relative to one another.
`
`[0023) Although the average torque value of the fourth experimental group was very similar to
`the average torque value of the control group, it was surprisingly discovered that the average
`angular deflection of the fourth experimental group demonstrated an increase of almost 250%
`relative to the average angular deflection of the control group. Additionally, the samples tested
`in the fourth experimental group demonstrated a cyclical fatigue of about 120 seconds as
`compared to about 30 seconds as demonstrated with respect to the samples tested in the control
`group. Also, the visual signatures of the individual data sets in FIG. 7 and FIG. 8 were more
`precisely aligned as best shown in FIG. 8. As a follow-up to the test results given above, more
`testing was performed with a focus on heating machined endodontic NiTi instruments as
`described above for about 120 minutes and gathering additional data.
`
`[0024] The purpose of the additional analysis was to build upon the experimentation discussed
`above in which the inventor was able to modify certain physical properties of Nickel~ Titanium
`through a specific heating process. Some goals for the additional tests are shown below in Table
`2.
`
`Page 6 ofl3
`
`
`
`Attorney Docket No. 6S46B.PV
`
`TEST ITEM
`
`I
`
`2
`
`3
`
`4
`
`s
`
`NAME
`Torque
`
`TABLE2
`CRITERIA
`
`I. 77 Minimum
`
`Angular Deflection
`
`360• Minimum
`
`ACCEPTANCE
`Must pass Minimum
`Criteria per ADA
`101
`
`Must pass Minimum
`Criteria per ADA
`101
`
`Cyclical Fatigue
`
`1 0-Series Equivalent Must be greater than
`Industry equivalence
`
`Flexibility
`
`1 0-Series Equivalent
`
`Must be less than
`Industry equivalence
`
`Clinician Feedback
`
`Inquiry
`
`Positive Feedback
`
`[0025] The additional testing followed the guidelines found in ADA no. 28 (sections 6.4 and
`6.5), ADA no. 100, and ISO 3630-1 (sections 7.4 and 7.5), the contents of which are
`incorporated herein by reference in their entireties. Cyclical fatigue testing is not an ISO
`standard test, but it has been utilized in the testing of rotary Nickel-Titanium instruments over
`the past few years. Such cyclical fatigue testing includes a motor unit 22 as shown in FIG. 9 set
`at, for example, about 300 rpm to simulate the speed of an instrument as used during, for
`example, a root canal procedure. A Ni-Ti test instrument is lowered into a simulated canal
`structure 24 which may be set at about 90° relative to the plane of rotation of the test instrument,
`until the depth of a calibration line along the test instrument is reached at, for example, about 19
`millimeters in reference to a first end 26 of the simulated canal structure 24. The amount of time
`the test instrument is rotated prior to breaking or otherwise failing is recorded so as to determine
`how long it took, under controlled conditions, for the test instrument to break.
`
`[0026) No less than twenty machined endodontic NiTi instruments which had been heat treated
`in a 500 oc oven for about 120 minutes were tested according to the criteria set forth above in
`Table 2. More specifically, the tested instruments were 10 Series™ endodontic files offered by
`
`Page 7 of13
`
`
`
`Attorney Docket No. 65468.PV
`
`D&S Dental, LLC of Johnson City, Tennessee, the files having a total length of about 25 mm, a
`working length of about 10 mm, and a and taper rate of 0.04 nun/mm. An important aspect of
`the method described herein is heat treating after machining of a NiTi dental instrument has a
`profound effect on the physical properties of the machined instrument. Table 3 below
`summarizes the test results.
`
`ITEM
`
`NAME
`Torque
`
`TABLE3
`
`CRITERIA
`
`1.77 mN·m
`Minimum
`
`RESULTS
`
`COMMENTS
`
`Worst Case
`4mN·m.
`
`Passed
`
`Passed
`
`Passed
`
`1
`
`2
`
`3
`
`4
`
`s
`
`Angular
`Deflection
`
`360• Minimum
`
`Worst Case
`s1o·
`
`Cyclical Fatigue
`
`10-Series
`25 seconds @ 90•
`
`Mean of 160.79
`seconds with a
`Standard Deviation
`of38 seconds
`
`Flexibility
`
`10-Series
`SOmN·m@4S•
`
`Mean of 18 mN·m
`@45•
`
`Clinician
`Feedback
`
`Inquiry
`
`Pros: Good Cutting
`ability, No breakage
`Cons: Too flexible,
`loss oftactile feel
`
`S pieces were tested
`for amount of torque
`needed to reach 45•,
`Passed
`
`Marginal
`
`(0027] The test results overall showed notable improvement in all categories listed in Table 3.
`
`The graph shown in FIG. 10 shows the twenty samples as plotted with respect to torque (vertical
`
`axis) versus angular deflection wherein 240 data measurements were taken per one 360° (axial)
`
`revolution of a tested sample. FlO. 11 shows trendlines plotted based on third order polynomial
`equations to best model the data results for each test sample. FIG. 12 shows the trendlines from
`
`FIG. 11 along with a bold trendline generated and plotted based on the average values of the
`
`twenty trend lines representing each test sample. Table 4 shows the model equations used to
`
`Page 8 of13
`
`
`
`Attorney Docket No. 6S468.PV
`
`generate each trendline in FIG. 11 as well as the equation used to generate and plot the bold
`trendline in FIG. 12.
`
`Coefficients as used in a third order polynomial equation f(x) = Ax3+Br+Cx+D.
`
`TABLE4
`
`Test
`Sample
`1
`2
`3
`4
`5
`6
`7
`8
`9
`10
`11
`12
`13
`14
`15
`16
`17
`18
`19
`20
`
`Coeffidents
`c
`A
`B
`D
`-0.000004 0.0271 4.4365
`-0.00000008
`-0.000005 0.0291 4.4036
`-0.00000008
`-0.0000001
`0.00002 0.0152 4.4996
`-0.000004 0.0346 4.7673
`-0.0000001
`-0.00004 0.0321 4.8333
`-0.00000002
`-0.000007 0.0195 4.7131
`-0.00000005
`-0.00000008 -0.0000006 0.0253 4.3494
`0.00000007
`-0.0001 0.0491 4.2493
`-0.000005 0.0314 4.2093
`-0.00000008
`-0.0000001
`0.00004 0.0182 4.3039
`-0.0000001
`-0.000007 0.0305 4.6517
`-0.000002 0.0252 4.6123
`-0.00000008
`-0.0000002
`0.00003
`0.03 4.6047
`-0.00000002
`-0.00002 0.0224 4.7004
`0.00000003
`-0.00006 0.0287 4.5002
`-0.00000007
`-0.000003 0.0243 4.5967
`-0.0000003
`0.00008 0.0209 5.063
`-0.00006 0.038 4.2322
`0.00000002
`0.00006 0.0285 4.7873
`-0.0000002
`-0.00000006
`-0.00003 0.033 4.9694
`
`[0028) Based on the results of the follow-up tests, the average torque value for the samples
`tested was about 4.57 mN·m. The average number of measurements taken prior to instrument
`failure was 372.5 which corresponds to about 1.5 full axial revolutions (i.e., 372.5 measurements
`+ 240 measurements per axial revolutions). The values are shown in FIG. 12.
`
`[0029) The results of the tests carried out above are promising because they demonstrate that
`heat treating an endodontic instrument to about 500 °C for about two hours or more after
`machining has taken place results in improved instrument flexibility. Such increased flexibility
`
`Page 9 of13
`
`
`
`Attorney Docket No. 6S46B.PV
`
`leads to an instrument such as the treated instrument 14' shown in FIG. 18 to more closely
`follow the natural root canal 12 of the tooth 10 and exhibit less lateral forces along the inner
`surface of such root canal 12.
`
`[0030) The improved cyclical fatigue measurements (as compared to untreated NiTi instruments)
`strongly suggests that endodontic instruments treated according to embodiments described herein
`will last longer and endure more stress prior to failing. This enhancement translates into less
`time spent extracting broken bits of instruments and more time accomplishing the goal of a
`particular endodontic procedure. Ultimately, such improvements will decrease chair time for
`patients, thereby increasing dental practitioner revenue.
`
`(0031] In one embodiment, a method is disclosed for treating medical instruments including
`placing a medical instrument into an environment held at least at about 450 °C to about 550 °C,
`more preferably from about 475 °C to about 525 °C, and most preferably from about 490 °C to
`about 510 °C for a period of from about 90 minutes to about 180 minutes and more preferably
`from about 120 minutes to about ISO minutes. The dental instrument is preferably an endodontic
`instrument made from at least about 50% of a superelastic alloy, and the instrument is preferably
`a tile, reamer, or a broach. The superelastic alloy is preferably Nickel-Titanium. The heat
`treated medical instrument preferably is placed in a metal pan with freedom of movement during
`the beating step.
`
`[0032) In a related embodiment, flexibility of an elongate machined medical instrument is varied
`along its length axis by heat treating only one or more discrete portions of the medical
`instrument. In the following examples, it is to be assumed that the medical instrument is an
`endodontic instrument including a working portion approximately I 0 nun in length, such I 0 mm
`length including a first end (tip) and a second end (rear), wherein the second end is adjacent a
`non-working portion of the endodontic instrument. The assumptions given herein are for
`illustrative purposes only and are not intended as a limitation on the technology as described
`herein.
`
`(0033] In a first example, an endodontic instrument made from primarily a superelastic alloy
`such as NiTi may be selectively heat treated along about 2 millimeters adjacent the first end (tip)
`
`Page 10 of13
`
`
`
`Attorney Docket No. 6S468.PV
`
`of the instrumen~ resulting in an instrument with a tip having enhanced flexibility with the
`remainder of the instrument remaining relatively rigid.
`
`(0034) In another example, an endodontic instrument made from primarily a superelastic alloy
`such as NiTi may be selectively heat treating a discrete cross section of a sintrument having a
`length of about 1 to about 2 mm located about 5 millimeters from the tip of the instrument. This
`will result in a relatively rigid tip, flexible middle portion, and relatively rigid end portion of the
`working portion of the instrument.
`
`(0035) In yet another example, an instrument is heat treated from the tip of the instrument to
`about 2 mm from the tip as well as heat treated from about 9 mm to about 10 mm from the tip of
`the instrument. This example would result in an instrument with relative flexibility near the tip,
`relative rigidity along a midsection of the working portion of the instrument (i.e., from about 3
`mm from the tip to about 8 mm from the tip), and relative flexibility from about 9 nun to about
`10 mm from the tip of the instrument.
`
`(0036] Other discrete treatment options are contemplated herein for treatment of specific axial
`cross-sections of an endodontic instrument to effect specific physical property alterations along
`the instrument's length as desired. The specific treatment may be accomplished using focused
`energy at certain points along an endodontic instrument and/or placing a resistance forming layer
`or layers on sections of an instrument that are not to be heat treated.
`
`(0037] The foregoing description of preferred embodiments of the present disclosure has been
`presented for purposes of illustration and description. The described preferred embodiments are
`not intended to be exhaustive or to limit the scope of the disclosure to the precise form(s)
`disclosed. Obvious modifications or variations are possible in light of the above teachings. The
`embodiments are chosen and described in an effort to provide the best illustrations of the
`principles of the disclosure and its practical application, and to thereby enable one of ordinary
`skill in the art to utilize the concepts revealed in the disclosure in various embodiments and with
`various modifications as are suited to the particular use contemplated. All such modifications and
`variations are within the scope of the disclosure as determined by the appended claims when
`interpreted in accordance with the breadth to which they are fairly, legally, and equitably
`entitled.
`
`Page 11 of13
`
`
`
`Attorney Docket No. 6S468.PV
`
`What is claimed is:
`
`A method for modifying a physical characteristic of an endodontic instrument, the
`1.
`method comprising the steps of placing an endodontic instrument in a heated environment
`having a temperature of from about 450 °C to about 550 °C for from about 90 to about 180
`minutes, wherein the endodontic instrument is made from at least about SO% by mass of a
`superelastic alloy.
`
`The method of claim 1 wherein the placing step further includes placing the
`2.
`endodontic instrument in a heated gaseous environment having a gas temperature of from about
`490 °C to about S 10 °C.
`
`The method of claim 1 wherein the placing step includes placing the endodontic
`3.
`instrument in the heated environment for a period from about 120 minutes to about 150 minutes.
`
`The method of claim 1 further comprising the step of machining the endodontic
`4.
`instrument to fonn a working portion prior to placing the endodontic instrument in the heated
`environment.
`
`The method of claim 1 further comprising the step of placing a resistance layer
`S.
`along a first section of the endodontic instrument prior to placing the endodontic instrument in
`the heated environment, wherein the resistance layer prevents the first section from undergoing
`heat treatment in the heated environment.
`
`The method of claim 1, wherein the endodontic instrument comprises a tapered
`6.
`endodontic instrument made of a nickel-titanium composition and configured as a file, rasp,
`broach, or other device for cleaning, scraping, extirpating, and/or debriding a root canal of a
`tooth.
`
`An endodontic instrument with modified memory characteristics, the endodontic
`7.
`instrument made by the method comprising the steps of placing an endodontic instrument in a heated
`environment having a temperature of from about 450 °C to about 550 °C for from about 90 to
`
`Page 12 of13
`
`
`
`about 180 minutes, wherein the endodontic instrument is made from at least about 50% by mass
`
`of a superelastic alloy.
`
`Attorney Docket No. 65468.PV
`
`Page 13 of13
`
`
`
`
`
`
`
`...:\.:§§...)..§....{..{.\}.::....\t\>.\x.§\).
`
`_\:§
`
`.»
`
`.i...x“
`
`.}.\}.......u.\\\\\\\\\\\~:..iii:.\\\
`
`V,
`
`\.
`§.\\
`
`X?xx.:...:t...>.::...x\\\\\..«2.......§.:..\..«.:3
`
`\'}
`....
`1
`\\
`
`,
`...........
`"\
`/
`
`18
`
`T‘
`FlG .. lB
`E‘
`EB
`
`10
`
`!0
`
`~t''····················
`
`\
`
`\\\\\.1:».
`
`\§.\.\.m
`
`' '
`
`\\:\\\§....\\.c
`
`\\\\\\.:.\\\.\\\\\\\§\h..\..\‘.{A.x...x\¥3<..
`
`
`
`
`
`\«...§§§§\§§...txxxx......
`
`.§.i\.>
`\\\\:
`
`w ‘W~
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Measmemem(2%peraxiai2”e*wla,ztian)
`
`
`
`
`
`5&0
`
`{'1
`KM}
`
`133zaa
`
`
`
`r .3»:
`‘mw’
`9‘
`
`‘
`
`
`
`I
`I
`I
`\
`\
`\
`\
`
`\
`
`\
`l
`* I
`l
`l
`~
`I
`t
`t
`l
`I
`t
`I
`1
`I
`t
`' \
`I
`t
`' ~
`\ ~ ' \
`
`\
`
`\
`l
`\ \
`
`t \
`1
`I
`t
`I
`\
`t
`'t
`I
`\
`\
`\
`\
`\
`\
`\
`\
`\
`\
`\
`\
`\
`
`\
`
`\ ' '
`
`\
`\
`
`' \ '
`..
`
`\t
`~ ;,
`\ "
`\ "
`'
`\ "
`
`
`
`
`
`
`\>\«\E«\~.«\«\\«~.\\\\
`
`)«
`
`
`
`0
`
`
`
`Measurement(24%peraxiairem§=ut%arz}
`
`0 g
`£308
`
`0
`7535.}
`0
`!'-
`
`~ -c
`
`0
`{$93
`0
`
`SM}
`
`!i'%«{1{}
`
`300
`
`
`
`
`
`mo
`
`«\~.\.~.-x>>:-or-no>>>x-:-to:-:-:-:-»»:-»:->:-:-:--*-:->:«c«\\\\\\\\\'<-:<c~:1:<-:<ccxwcwmxx-.-.-.-.-.~.~.\~.-.\\~._\._._._
`
`3..
`
`.
`
`93‘
`
`£..u"‘§
`
`t"§“$
`
`f"\‘
`
`if}
`
`>:'*5
`
`
`
`
`
`
`
`
`----------------~
`
`>·
`
`:··
`
`*-----------------------
`
`'t(lfo(' ...... ~ .............. "f+l' ...... '+f*~"'"""~
`
`a
`0
`f"..
`
`0
`0
`V).
`
`0 a
`
`t.tl
`
`0
`0
`<::::!'
`
`0
`0
`N
`
`0
`
`
`
`
`
`0
`0
`0'>
`
`8%}9
`
`.70{Zr
`
`Efiif}
`
`0
`Efii}
`0
`l.f"1
`
`0
`fiflii
`0
`~
`
`0
`3:229
`0
`M
`
`C• a
`Zfiéffi
`N
`
`1.535’)
`
`{'1
`0
`
`·------------------------
`
`----------------
`
`
`
`£3?
`2»24
`
`-------------------------
`
`
`
`51.1%
`
`Vi‘
`
`U“)
`3
`
`{Y3
`
`if’:
`Z
`
`\’‘'’-3
`
`L93
`1
`
`‘z-~¢
`
`m
`{ES
`0
`
`0
`
`
`
`{mwmm} anisgcgi
`
`
`
`
`
`
`
`
`
`
`
`
`
`Wiiaasmremem€246perMia!rmm§z2tia:':}
`
`
`
`0
`0
`0
`1""1
`
`0
`0
`0'=
`
`a
`0
`00
`
`0
`0
`~"--·
`
`-c
`
`0
`
`························································································································~--
`
`{tU·NW) anbJOi
`
`
`
`.._...,, --.......
`
`............................................‘............................................................................................................................................‘‘‘‘..‘.‘‘.‘.....‘.....‘‘‘‘.‘..‘‘.‘‘....‘‘..........................................................................................................‘‘‘.‘.‘.............Lm.w...w.§.A
`
`'
`t :
`t ~
`l ~
`
`<
`
`l ~
`
`l :
`\ ~
`
`~. \ \ ..
`t : l
`~ \.\·.
`~ \ .\·
`\ \\
`\. :.· ·~·.
`\ ~
`\ ~
`\ \~·.
`\ '. ..
`\\~.
`\ ·\\
`\
`\
`\
`\
`\
`\
`
`< ' t
`I ' t
`
`I
`
`* t
`
`t
`I
`l
`1
`
`\
`\
`t
`\
`' 1
`\
`\
`\
`\
`\
`\
`\
`\
`\
`
`' \
`
`\
`\
`\
`\
`\
`
`' \
`
`\
`\
`
`' \
`
`\
`
`\
`\
`\
`
`' \
`'
`.,
`·-..
`"\
`·.
`\
`~-
`'·, '
`' ·. \.
`
`\
`
`.... ~.:
`
`0
`
`0
`0 ,.....,
`
`0
`0
`Cl'<
`
`.13:gmSm.GE.mamcumQ03gmcomQ3Q
`
`0
`
`
`
`
`
`M§mmE>m.mwmwxmEmmwmwwamwmmwxmmmmmw
`
`\
`
`....................................................................................................................................................................................................................................................................................................................................................
`
`
`
`FIG,. 9
`
`22
`
`26
`
`
`
`.,\\\\V\\\\§\.\\\\\\\\.\\\\\.\.\\x.\
`
`,&\\o\\\\\V\xVx.\k..\.\\\\\,«M¥+§\\x~v\¢\\\
`
`
`
`~$\\\\V\.W..u\.u%
`
`\\\\\\s..&\~V\.u.\\
`
`\\x\«\\\\\\»\
`
`mam
`
`mmmmmmQmmmammmw
`
`0 a
`N
`
`a
`mew
`0
`rl
`
`
`
`
`
`mm®$§m..sm.mmmwxm“mamwmwMfimfimhmmmmwg
`
`E.mw.§
`
`ww
`
`{X}
`
`{Q
`
`M
`
`Q
`0
`
`a
`
`{mamas} ¥3¥¥b.i£3g__
`
`
`
`
`
`
`
`
`
`~
`~
`
`W.M.M%¥mm
`
`" r~ v
`~
`~
`
`0
`0
`ul
`
`0
`0
`"Cf
`
`0
`If)
`{'()
`
`
`
`mam.amwnewmmmmammamQQNEmQ3,omQ
`
`0
`0 m
`
`0
`~t)
`N
`
`0
`0
`N
`
`0
`!..<"\
`rl
`
`0
`0
`..-i
`
`{aunmzu} aiwizamga
`
`0
`
`0
`
`-t:
`0 ·-~ ::;
`0 > (JJ
`~ -ro ·-X ro
`
`
`
`~· cu
`0..
`0
`~
`
`N -+<' c
`
`(1)
`
`Mgamuswmnmhmmwxm(“mmmwmw§§E$:mm,m§
`
`
`
`E
`
`QJ
`t...
`::l:
`Vl ro
`Q)
`2
`
`
`
`' . '
`x>w4xx
`
`
`
`»e«..x¢....v.........»..,.<<exx
`
`,.
`
`.>ex_
`.»e.+¢¢x<x...x..w
`< . .
`
`' '. ·~ +
`
`~
`
`" ..
`)>""
`..~··
`.: .....
`.,.:
`~ ! t
`
`ex,x>
`
`.~ "' ... ,,,
`... -~·· ><I
`.,.) ,,,
`~¥ ,
`
`t ~+
`
`......... .. .,
`~~" ... .,
`.... ,.
`~,
`t.
`'·' h
`',: .. ~
`\"';,.
`... "" ...... _,
`~\.
`
`-~~-i' ... t .. ~
`
`!!
`.s“
`< ~( ""'
`···.S""'
`...
`...... -~
`-"- 4-
`·~
`•:::: ..... : · · · · ; ~--: W•'
`$ ~ .... ~ )
`
`:;:Jl ~ ~
`""'"''""'
`,:·:}_;,;
`
`~, ~ ~
`
`
`>¢xvM%¢w¢3A¢o¢+¢:w¢>>>>.xx
`
`ei>+fit£«e1o¢¢¢@¢3v++vo)a.
`
`....e..
`.xx.xv...xx.x
`« ..
`
`u.
`.»x.
`.................................
`
`"'-'·
`
`·.-....
`
`xxx
`
`,-,x»
`
`xxiuéw.x...x..e..Y.....x1xxx.x+..sx<¢..
`ssaewwuxxxaan;\\\vvv:)\i(¢@!ve
`
`'' ' ' '.
`' ' < < ..
`
`M§$3
`
`
`
`...x.xxx.xx.xx»\\\u.\\\\\\..x.xxxxxx..xxxxxx.xx.\\\:5
`
`0
`.....
`'~">
`~~1
`
`0
`0
`(¥)
`
`mmmom3.Nmammm;
`
`0
`!..{'\
`N
`
`a
`0
`N
`
`0 tn
`x-i
`
`0
`0
`'C"""l
`
`0
`
`ma
`
`{~'\
`iwm
`.mmm,NW
`
`
`
`mmmm.3§...$wmwxmEmmwmw§m..§m§w§_§
`
`·-t:
`
`0
`"*J
`:J
`0
`::.0
`())
`lo-
`
`
`
`ro
`X ro
`QJ n
`0
`q"'
`
`~
`
`N -~'""' c
`
`();;t
`
`E
`il1
`~-
`~
`~..~ ro
`())
`2