GLASSY CARBONS Semi-Annual Progress Report for the Period June 1, 1972 to December 31, 1972 January 1973 ARPA Order Number: 1824 Program Code Number: 1D10 Contractor: The Regents of The University of Michigan Effective Date of Contract: 1 June 1972 Contract Expiration Date: 31 May 1973 Amount of Contract: $162.580 Contract Number: DAHC15-71-C-0283 Principle Investigator: Professor Edward E. Hucke Department of Materials & Metallurgical Engineering The University of Michigan Ann Arbor, Michigan 48104 (313) 764-3302

The views and conclusions contained in this document are those of the author and should no be interpreted as necessarily representing the official policies, either expressed or implied, of the Advanced Research Projects Agency or the U.S. Government.

TABLE OF CONTENTS Summary......... v I. Introduction............ 1 II. Materials Preparation........ 5 III. Structural Studies......... 8 A. Solid Structure........ 9 X-ray Studies.... 9 Electron Microscopy and Diffraction... 11 Thermodynamics..... 22 B. Pore Structure.......... 32 Small Angle X-ray Scattering...32 Experimental Procedure...33 Results........ 34 Electron Scanning Microscopy...... 37 Pycnometry.... 38 Surface Area.......... 39 Mercury Evaluation..... 39 IV. Property Evaluation......... 40 Hardness............ 41 Compressive and Ultimate Tensile Strength 41 Sonic Modulus and Internal Friction... 45 Electrical Resistivity...... 47 References........49 Appendix............. 51 iii

SUMMARY A large number of glassy carbon samples was produced by controlled pyrolysis of furfural alcohol resins, examined for structural differences, and evaluated for physical and mechanical properties. It is concluded that glassy carbon is a family of materials whose properties can be varied over a significant 0 range, depending both on the small scale (2-50A) carbon structure, and the amount and distribution of porosity which may be present in substantial amounts. The combination of availability, chemical stability, low density and high strength make glassy carbons look promising for mechanical applications, particularly at very high temperatures. In terms of strength per unit weight, glassy carbons compare favorably with the best available materials even at room tempero ature. Very fine pored (<100A) glassy carbons have been produced in section thicknesses of 2 inches in processing times of six days, which significantly increases the range of potential application. The carbon's fine structure determined by electron microscopy, electron diffraction and X-ray diffraction is not homogeneous on a size scale below 100 Angstroms. The material is 0 paracrystalline with the crystallite size ranging from 10-100A depending on processing, and with some very crystalline features 0 occasionally existing in sizes up to 500A. v

A thermodynamic method has given results yielding a direct measure of the degree of order in terms of the configurational entropy and enthalpy relative to crystalline graphite. Helium, xylene, mercury intrustion, small angle X-ray scattering, surface area analysis, and scanning electron microscopy show the pore structure of glassy carbons may be either 0 isolated or interconnected, and in a size range from 5A to 50 microns. Mechanical strength has an inverse relation to the pore size. The pore structure allows a decrease in density, as well as the opportunity to vary mechanical properties and provide chemical filtering and absorption appliances with substantial strength. vi

GLASSY CARBONS I. Introduction This report covers work carried out during the period June 1972 to December 1972. Results of the previous contract periods are summarized in two previous semi-annual reports.'2 Since various property evaluations are being carried out simultaneously, the data tables included in this report are cumulative and have been revised to reflect additional samples as well as corrected in certain instances where samples were either improperly identified or errors in data reduction occurred. Complete data tables are given in Appendix A. Glassy carbons have already been shown to have an unusual set of properties, particularly with respect to inertness and high strength to weight ratio. These attributes, together with the ready availability and high temperature capability of carbon naturally lead to potential applications in a wide variety of extreme conditions, such as reentry shields. Aside from mechanical applications, the unusual inertness in the human body has lead to a wide variety of biomedical applications, while its electrical properties have shown experimental promise as a semi-conductor switch, and its molecular sieve properties suggest applications in chemical separations. Glassy carbon is still a new material and at present is -1

costly and available only in thin sections. The high cost and section limitation both stem from the need to use very long pyrolysis cycles in order to obtain material without cracks. A major objective of this research has been to achieve larger section bodies with rapid processing times. While all of the glassy carbons made from a variety of polymers and gaseous precursors are hard, strong and light, many subtle variations exist and considerable tailoring of properties is possible. A major difficulty in comparing the various carbon materials is that no simple criteria are available to distinguish one from the other. In general, many of the physical and mechanical properties show significant differences and one can give a comparison of one material with another only by specifying a complete property set. All of the properties derive ultimately from the structure and therefore it is important to be able to elucidate, control, and specify the structure of the material. The lack of a well-defined crystalline structure severely complicates matters since not only are the usual microstructural features (.1 to 100 microns) important, but also variations in the ultrastructure (3 to 100 Angstroms) are encountered. Even a seemingly straight-forward property such as real density becomes elusive because it can vary on size scale 0 of the order of 50A. With an understanding of structural variations possible, extension in the range of properties achievable can be made. From data previously available in the literature and the early -2

results of this program2, it has become obvious that "glassy carbon" is not a single material, since even though it contains essentially only carbon atoms, its structure can be varied at all size levels. It seems more appropriate to think of glassy carbon as a material that may have short range atomic coordination with a variable state of crystallinity; but in addition, where rather large fractions of thermally stable voids can be arranged at size levels from 5 Angstroms to 50 microns. This accounts for the extremely wide variation in properties that can be achieved. The incorporation of voids into materials is not unique. However, it is unique to have up to 30% void remain stable in material at temperatures close to sublimation when the pore size is well below 100 Angstroms. Glassy carbons possess some crystallinity on a scale of the order of 100 Angstroms or less, but the perfection of the crystallites is very poor by usual standards; and while the crystalline perfection may improve after heating to very high temperature, a well-defined graphitic structure is not achieved without unusual methods. The structure is better described as para-crystalline in the sense used to describe certain polymers. In fact, the glassy carbon structures are best considered polymers with vanishing contents of other than carbon atoms. The carbon structures are related to the polymer structures from which they evolve during pyrolysis. This observation follows from the differences obtainable in structure and properties of carbons after heating to 3000~C by merely changing the thermal history -3

of the polymer in a temperature range below 100~C where polymer structure is being formed. Thus, even though most of the atoms present in the precursor polymer are later removed, the resulting carbon inherits part of the structure. The present study is largely concerned with structures obtainable together with the simultaneous measurement of certain key physical and mechanical properties. It is desired to achieve in different samples as wide a variation in structure and properties as possible. The structure is being investigated from the viewpoints of the solid structure and the pore structure, which of course are related. Since significant differences can be induced in both over a size range of more than four orders of magnitude, no single technique is sufficient. Instead, combined techniques must be used. Each is discussed in detail in the following sections of the report. Representative property measurements are being carried out in conjunction with the structural examinations. Due to the large number of samples processed, complete structural and property evaluations are not attempted on every sample. Apparent density, real density, wide angle X-ray diffraction, scanning electron microscopy, and strength measurements are made on every suitable sample. Small angle X-ray scattering, selected area electron diffraction, transmission electron microscopy, thermodynamic analysis, surface area analysis, mercury porosimetry, electrical resistivity, hardness, modulus of elasticity, and internal friction are carried out on a selected -4

small number of samples. II. Materials Preparation During this report period over 500 samples of glassy carbon were prepared with over 95 different processing conditions. The work has continued to concentrate on furfural alcohol and a furfural alcohol resin, Durez 16470* as the carbon yielding material, with para-toluene sulfonic acid (PTSA) as the polymerization catalyst. However, a limited number of samples has been prepared with other type resins (Varcum 8051 and 4048)** and other catalysts made experimentally by the Quaker Oats Company. While glassy carbons are obtained in all cases, the yield of good material and response varies for each system. Thus far, the best results have been obtained with the Durez-PTSA system, although this may be only due to the greater experience with this system. Catalyst levels from 2 to 20% by weight based on the monomer or resin content have been explored. Temperatures for addition of the catalyst and subsequent curing time and temperatures have been varied from several minutes to several weeks with temperatures from -11~C to 150~C. In all cases where a particularly interesting set of properties has been found, a duplicate set of specimens has been made to check reproducibility. In general, reproducibility is fair, but only if meticulous care is exercised to exactly reproduce all conditions. Standard sample cylinders * Hooker Chemical Company, North Tonowanda, New York **Reichhold Chemical Company, White Plains, New York -5

approximately 3 cm in diameter and 20 cm in length have been adopted. Samples up to 15 cm in diameter have been produced from coarser pored material, while a few samples of 5 cm have o been made from very fine pored (<100A) material. The latter sample is far thicker than any other similar material previously reported even though its pyrolysis time of 6 days is much shorter than usual commercial practice. The yield of crack free material has continued to improve due mainly to increased care in catalyst addition and prevention of trapped bubbles prior to and during casting. The presence of bubbles has been found to cause cracking in the subsequent pyrolysis of the samples. In most cases, it has been possible to perform a reduced pressure de-bubbling operation after addition of the catalyst. In order to yield good material, it has been necessary to perform the hardening of the resin systems with a minimum temperature gradient throughout the piece, which often requires cooling after addition of the catalyst. The length of time curing, curing temperature and catalyst level have been varied over wide ranges. The single-most important factor in obtaining crack free materials in pyrolysis is obtaining a uniform slow heating rate. While heating rates have been varied from 5 to 50~C per hour in the range of room temperature to 1000~C, the yield of crack free material is much greater at the slower rates. Rates up to 200~C per hour appear to cause no difficulty in heating material previously pyrolyzed to at least 700~C. Both flowing nitrogen and -6

reduced pressure pyrolysis have been employed. Thus far, flowing nitrogen appears to yield less difficulty with respect to cracking. On selected samples, carbon recovery and shrinkage data have been gathered. In both cases the data are comparable with those of the literature, namely a carbon recovery based on the total resin weight of about 55% and linear shrinkage of about 29%. However, differences in both shrinkage and recovery of about 10% can be noticed with varying of curing and pyrolysis schedule. Inhomogeneities of about 1p in diameter in the starting resin were noted in the previous report2. These regions carry through the pyrolysis and cause non-uniformity in the final structure. At present no completely satisfactory method has been found for eliminating this problem, although filtering the starting resin has made an improvement. Rather subtle differences exist in the cured resins which result in different properties after pyrolysis. Thus far no satisfactory means for quantitatively studying the resin have been developed. Exploratory work using scanning calorimetry has been initiated in an effort to see if the differing final results can be detected from the thermal changes occuring in the polymer stages. The single-most important processing variable is the maximum pyrolysis temperature (HTT) which has long been known to affect the structure and properties. However, all the other processing variables have some influence even though at this time the data show no clear-cut correlations. Part of the difficulty -7

in finding a correlation is undoubtedly due to the fact that the exothermic polymerization causes heating of parts of the sample above the temperatures of intended control. It is also probable that many of the effects noted in mechanical properties may be due to the existence of very fine cracks or possibly residual macroscopic stresses in specimens that appear to be macroscopically sound. In this case, a particular processing change may appear to cause a large effect on the properties, but may only aid in yielding a more flaw free sample. However, it is difficult for example, to understand how this explanation can be applied to the observed differences of 20% in real density (-325 mesh powder) with different curing schedules. III. Structural Studies While the eventual goal of this study is to correlate structure at various stages of the process with properties, the results thus far are largely drawn from samples taken at only two processing stages. The first stage corresponds to a maximum temperature exposure in the range 650-1000~C, while the second stage is that formed at about 2000~C. More recently, samples have been examined at HTT between 1000~C and 2300~C, since for given processing conditions maximum values of mechanical properties were noted in this range. The techniques chosen for structural examination fall into two broad categories with respect to the information yielded. The first yields information predominantly about the state of the -8

solid making up of the structure, while the second deals mainly with the void structure. In the first category this study is employing bright field and dark field transmission electron microscopy, electron diffraction, wide angle X-ray diffraction and scanning and electron microscopy. The last two methods also yield information on pore structure. Additional techniques used to establish the pore structure are small angle X-ray scattering, helium pycnometry, mercury porosimetry, and surface adsorption. An attempt is also being made to gain structural information through a precise measurement of the thermodynamics of the equilibrium Cgraphite = Cglassy Since the effort required to carry out the above techniques varies substantially, a complete set of data will be collected on only a limited number of samples after screening with more routine tests. A. Solid Structure X-ray Studies Several useful measures of the state of non-graphitizing carbons can be derived from wide angle X-ray diffraction. The usual data for d(002), L, d(10), and L have been measured for c a a sample from each processing condition with the results reported in Table 1 of the appendix. The procedures are the same as previously reported2. The "crystallite size" parameters, Lc -9

and La are in reality only line broadening parameters and can not be literally interpreted as the size of graphite crystals, since the analysis considers only size broadening of highly crystalline material and ignores strain effects and the possibility of a distribution of layer spacings. These parameters are useful for comparing different samples of glassy carbon and correspond roughly to a paracrystalline size determined by electron diffraction. The results obtained to date are similar to others in that they show an increasing Lc and La, and decreasing d(002) as the pyrolysis temperature is raised. These results are consistent with the idea that the structure is based on imperfect layers from 15 to 50 Angstroms thick with a layer spacing significantly 0 larger than graphite (3.35A). As previously reported, a large number of samples, but not all, show multiple reflections within the (002) line giving the impression of a multiple phase material. These samples have been designated as 2P, 3P or NVS in Table 1 where other than a smooth broad 002 peak exists. These results give strong support for the behavior postulated by Houska and Warren3 for carbon blacks where they concluded nearest-neighbor pairs of layers assume the ordered graphite relation independently. Layer spacings o o of 3.35A and 3.44A exist corresponding to ordered and disordered pairs, respectively. In the present study the 2P or 3P samples show very good agreement with these values. There is a strong tendency toward multiple reflections with higher pyrolysis tem-10

perature, and some correlation with longer curing times and higher catalyst concentration. However, there are many reversals and no satisfactory reason can now be offered to explain why this behavior is sometimes present and sometimes not. It is possible that sharp lines are always present in the (002) but that their intensity is too low to allow resolution in all but exceptional cases. The electron diffraction results confirm this finding. The only clear-cut correlation between the X-ray data and any processing variable or measured property exists with HTT. While additional correlations may be possible, it appears at present that the X-ray data are not very sensitive indicators of the structural differences that influence the measured properties. The table below indicates the relation of Lc to pyrolysis temperature. HTT ~C Lc, Angstroms 700 15-18 1300-1450 18-26 1500-1700 19-29 2000-2300 25-110 However, for a given HTT, a variation outside the experimental uncertainty exists for samples with no other apparent processing differences. Electron Microscopy and Diffraction Transmission electron microscopy (TEM) is being used to examine the microstructure of selected glassy carbon samples. -11

Samples for direct TEM and selected area electron diffraction (SAED) are prepared essentially the same way reported earlier1'2, except that now ultrasonic treatment of powder is done for 5-10 minutes. This results in smaller particles which result in better micrographs. However, further improvements in the method of sample preparation are still being explored. Bright field electron micrograph obtained at magnifications of 36400 to 66300 revealed similar structural features to those reported previously. However, in many samples cylindrical features and evidence for oriented texture have been seen. In general, 0 irregularly shaped platelets 150-500A in diameter were observed. The granular texture is more distinct in samples heat treated at higher temperatures in agreement with earlier findings. There is considerable variation in the size of platelets and granular texture within the same sample. The characteristic platelet and granular texture diameters are listed in Table 2. Figure la, taken from sample 321-31D(2300) shows granular texture very clearly but the platelets are not very distinct. Similar features are also visible in certain parts of Fig. 2 taken from sample 317-48(2000). The granular texture size recorded in Table 2 is generally more than'Lc', the crystallite height, and less than'La', the crystallite diameter, as measured by X-ray broadening. This suggests that the texture represents domains of paracrystalline material. The variation of size of the granular texture is in agreement with the fact that the Lc and the La obtained from X-ray line broadening are only average values of -12

Figure la. Sample 321-31D(2300). Typical granular texture characteristic of bulk of the material. The platelets are not very distinct. -- Figure lb. SAED pattern from upper left corner of the above. Both (002) and (100) contains small spots. -13_ — ~ _0O~ -13

Figure 2. Sample 317-48(2000). Typical platelet and granular features are shown. In addition, cylindrical features are also shown by arrows. -14

Figure 3a. SAED from 317-49(2000). Streaking can be seen in (100) and (110) halos indicating oriented texture (pattern was exposed thrice to bring out different rings and streaks). Figure 3b. SAED from 321-31C(2300). Elliptical diffraction pattern characteristic of oriented texture. (002) planes are inclined at an angle of 20 degrees from the beam. -15

(a) Figure 4. 321-31C(2300). (a) Very small granular texture can be seen on the upper right corner. SAED from this was typical of amorphous material. The region on the left side of the figure is more transparent and smooth. SAED of this region revealed that it is mainly graphite as shown in (b). -16i < i!~iii!ii < i!1 -1 6

(a) 500A the SAED of (c) was taken. -17-1 7

500 -a Figure 6. Sample (321-31D(2300). Dark field micrograph taken from (002) halo of SAED shown in Fig. 3b. -18

crystallite size and considerable variation might be present. In some regions granular texture is extremely small and thus not very distinct. Micrograph of one such region is shown in Fig. 4a. These regions are generally highly crystalline as indicated by their corresponding SAED patterns. Fig. 4b is an example which was taken from the left side of Fig. 4a. The (002) ring of this pattern is very weak in intensity and spotty, suggesting that the basal planes are perpendicular to electron beam in most of the region. The d(002) of the region is 3.35 indicating presence of graphite crystals in the region. Another exceptional feature reported earlier for 318-29 (2000) and 311-19(750)2 has also been observed in the samples 317-48(2000), 317-49(2000) and 321-31C(2000). In these samples long cylindrical features are clearly visible as can be seen in Fig. 2 (indicated by arrows). Selected area electron diffraction patterns, in most of the cases, showed three diffraction rings corresponding to (002), (100) and (110) reflection (see Fig. lb and 5c). However, in some cases many additional rings corresponding to higher reflections were also present. The sharpness of the diffraction pattern varied from area to area within the sample. This indicates that a particular sample is non-homogeneous on a microscopic level as would be expected for paracrystalline material. In addition to the diffraction rings, some of the diffraction patterns contained diffraction spots on the rings (see Fig. lb and 4b). In some cases diffraction spots were slightly -19

displaced from the rings corresponding to smaller d(002). The presence of spots on the rings suggests that larger crystals are present in that particular area; while spots corresponding to smaller d(002) suggest the presence of more perfect crystals. 0 These crystals have d(002) greater than 3.35A which indicates that they might correspond to the second phase seen by X-ray diffraction. Figure 4b shows the diffraction pattern from 32131C(2300). The area from which this is taken is very graphitic o as suggested by the d(002) which is 3.35A and six spots on the (100) ring. The (002) ring consists of very small spots of low intensity while the (100) ring is very sharp as would be expected if most of the crystals were oriented with basal planes perpendicular to the beam. Figure 3a shows SAED pattern from 317-49(2000). The (100) and (110) rings contain "streaking", i.e., tangential straight lines on these rings. The streaking is caused by the crystals oriented with their (002) planes parallel to the beam. 4" Figure 3b shows elliptical diffraction patterns from (100) and (110) reflections. However, the (002) reflection gave a circular halo but cannot be seen in the figure due to its very low intensity. The distribution of reflections along ellipses is characteristic of an oriented material struck by a beam at an angle to some welldeveloped plane.5 In the above case, the (002) planes are tilted at an angle of about 20 degrees from the beam. Electron diffraction spots on the SAED patterns have also been observed in 312-31(2000) which was originally identified to -20

be single phase according to X-ray diffraction study. This suggests that the so-called single phase type samples may contain other phases, though in minute amounts. However, no spots were detected in sample 321-31D(2300) which was also identified as a single phase type from X-ray study. In general, 3-phase type samples show more diffraction spots and more crystalline areas compared to other types. This was seen clearly in samples 317-33 (2000), 317-48(2000), 317-49(2000), 318-12(2000), and 321-31C (2300), which were 3-phase type, and 312-31(2000) and 321-31D (2300), which were single phase type. Ultrasonic treatment of samples before depositing them on the microgrid has resulted in better dark field micrographs from (002) reflections and made it possible to get some micrographs from the (100) reflections as well. However, dark field micrographs from the (100) ring is usually extremely poor in intensity requiring high exposure times. Dark field micrographs, obtained from (002) reflection, reveal as bright spots the regions or crystallites giving rise to the reflection. Accordingly, the diameter of these spots is equivalent to the crystallite height, Lc. Similarly, dark field micrographs from (100) reflection represents the crystallites giving that reflection. Thus, the diameter of the spots are equivalent to'La'. Table 2 lists the diameter obtained from these micrographs for different samples. It can be seen that the diameter from (002) dark field is in fairly good agreement with the X-ray'Lc'. But the diameter obtained from (100) dark field -21L

is generally very much higher than La. A possible reason for this is drifting of the sample caused by long exposure times of up to 1 minute needed to record these micrographs. Figure 6 shows the dark field micrograph obtained from the (002) reflection from the sample 321-31D(2300). Table 3 shows that average d(002) and d(10) spacings from SAED agree fairly well with the values obtained from X-ray diffraction. The most common error in measuring these values was perhaps varying contraction of films and thus a varying camera constant for every sample. The (100) ring of graphite powder was used to calibrate the microscope for every run. Yet a further check was made with the (100) reflection from the sample itself since ideally d(100) from the sample should always yield a value 0 close to 2.13A. Often additional diffracting maxima were observed, which sometimes are not indexable. Further detailed investigation is being done to find if they are not caused by impurities in the sample. However, they may be due to one or more of the crystalline forms reported by Whittaker.6'7 Thermodynamics Work has progressed in the program for direct determination of the thermodynamic properties of the following equilibria: Cgraphite = Cglassy (1) Cgraphite + C02(g) = 2CO(g) (2) -22

CO(g) + %02(g) = C02(g) (3) C02(g) + H2(g) = CO(g) + H20(g) (4) Results are available from at least one run on each of the above equilibria. The primary interest lies in precise measurements of reaction 1 for various types of glassy carbon, while the others are of interest as supplements to already available data. It has been previously noted8'2, that values of the free energy for reaction 1 versus temperature can be used as a direct structural measure of the disorder of a particular carbon structure relative to graphite. Available data for the heat capacities of graphite and various glassy carbons9'10l11 show that any vibrational contributions to the free energy in the range of temperature of interest will be 10 cal/mole or less, which is completely negligible. Therefore, the measured differences can be considered wholly configurational and separated into enthalpy and entropy terms. Disorder such as mixed bonding or strained bonds will cause changes in the configurational enthalpy and a definite increase in the configurational entropy, which can be directly interpreted as a numerical disorder parameter. Such techniques have already been applied in the case of polymers to determine degree of crystallinity12, where configurational (residual) entropies up to 5 cal/ mole-~K are found. Configurational enthalpies of %1500 cal/mole have been previously measuredl3 between glassy carbon and graphite by heat of combustion. Using another reaction, rather large energy differences have also been measuredl4 between graphite in -23

normal and rhombohedral stacking. In addition, Gordon 5 has pointed out from an examination of the discrepancy between experimental determinations of the equilibrium constant for the producer gas reaction and values derived from heat of combustion and spectroscopic data that a residual entropy of.5 cal/mole-~K may exist in near perfect graphite. The proposed cell method should be considerably more accurate than the previous methods and yields both the AH and AS. A rather extensive set of check runs has been made in order to insure precision and otherwise check experimental procedures. A series of runs previously reported2 was carried out on oxides (NiO, FeO, CoO, Nb02, Nb205, C02, H20) with known thermodynamic properties in order to verify cell configurations, electrical and temperature measurement techniques, gas train functioning, thermal diffusion effects, and solid electrolyte composition. In all cases, extremely gratifying confirmations were found. Measurements have been carried out with two entirely different cell techniques; however, at this time, not for the same sample. The first type uses a molten salt, CaCl2 with CaC2 dissolved, and involves reversible transfer of carbon directly from one electrode to the other. While the method is straight-forward, the useable temperature range and other experimental difficulties cause limitations. Also, the details of the charge carrying species are less certain since only one previous study16 has been completed. However, Fig. 7 shows -24

pt/graphite/Ca C2(Ca C12)/glassy carbon/pt e E -800- Graphite -Glassy Carbon oC 0 -400 -~400~~?^// Glassy Carbon / 1 /321-7-1600~C E - Gat 90e1000,,9 H 80 cmole o O / Temp. OC Graphite 321-7-14000C a 400 AH = 8,909 col/mole / AS = 7.45 e.u.' / 321-7-1600 ~C A AH = 752 cal/mole Q 800_ A S = 0.65 e.u. Figure 7. -25

the results obtained for two portions of a glassy carbon sample differing only in the HTT, i.e., 1400~C vs. 1600~C. The data, as expected, fall on two straight lines which yield the results below Sample AH, Cal/mole AS, Cal/mole-~K 321-7(1400~C) 8909 7.45 321-7(1600~C) 752.65 The results, especially for the 1400~C sample are remarkedly high but are quite consistent with the expected behavior of less disorder after higher treatment temperatures. While this cell technique appears feasible, it will be held as an alternative and check procedure since the solid electrolyte technique seems more versatile. The solid electrolyte cell involves measuring the difference in 02 pressure existing of opposite sides of the electrolyte where this pressure is additionally constrained to be in equilibrium with CO and CO2 and solid carbon. The details of analysis have been presented elsewhere. 82 If a difference in PO exists between the two sides at equilibrium with the same temperature and total pressure after starting with either CO or CO2 or 02, then it can only be due to a difference in the activity of the two carbons. While the equilibrium value may be the same regardless of the starting gas, the rate may be quite different. In order to check the functioning of the cell, several runs were made with Pt only on both sides and then with graphite on both -26

sides in order to verify that no stray EMF was involved. The cell voltages measured were always less than.1 millivolts. The graphite used in all the runs to date has been a common electrographite (UCC-grade CS) and will be replaced by a carefully selected graphite standard. The cell was next run with air on one side so that the measured EMF is a direct measure of reaction 2, where the activity of the solid carbon (graphite) is unity by definition. The results are shown in Fig. 8. The agreement is extremely good, since the experimental points lie very close to the best known line and well within the scatter band for the previously available data. Even more refined measurements over a wider temperature interval will be made on the graphite standard. The cell was well-behaved with equilibrium established within several hours. Equilibrium could be approached from both directions and the same value obtained after thermal cycling. The cell voltages have been measured with a high impedance Keithley differential voltmeter, a Keithley electrometer, and a calibrated L&N potentiometer, purposely set to polarize the cell in opposite directions. These experiments show the cell EMF to be reproducible, sensitive, accurate, reversible, and sign consistent. The next series utilized graphite in one compartment and various glass carbon solid discs in the other. The glass carbons are weighted for total carbon loss and both sides are exposed to pure CO2 after evacuation. Companion runs on the same samples starting with 02 both before and after CO2 exposure are planned. -27

C (s) + C02() = 2C (g) / Total Pressure = 0.976 atms / pt/Air(g)/Zr02-CaO/graphite(s),CO(g),C02(g)/pt / -11,000 / / / / / / // / ) -9,000 / // / / / 0 L / / / * Present Study < _7000 / / / -- Calorimetric Data 7000 / / / -- Scatter Band / / / -5,000 / / 800 850 900 950 1000 TEMP ~C Figure 8.

The results for portions of a glassy carbon pyrolyzed to 700~C and then vacuum heated for 1 hour to 1060~C, 1243~C, and 1800~C are given in Fig. 9. Again, as expected, the data fall on good straight lines giving the following values for AH and AS which are shown in a provisional plot in Fig. 10. Specimen AH, Cal/mole AS, Cal/mole-~K 321-13(1060~C-Vac) 9029 8.66 321-13(1243~C-Vac) 4934 4.70 321-13(1800~C-Vac) 3689 4.60 The rate of approach to equilibrium at the higher temperatures was rapid, but took 2 to 3 days at 650~C, the lower limit for the electrolyte. Future runs call for use of crushed samples to hasten equilibrium. The EMF's of up to 40 millivolts were stable, sensitive, reversible and could be approached from heating or cooling. There can be no doubt that replacing graphite with glassy carbon caused a dramatic change in cell voltage. While the data are yet too few to draw sweeping conclusions, they do show the expected trends. Again, the magnitudes are embarrassingly high. It is interesting to note that the configurational enthalpy drops steadily with HTT while the order increases rapidly from 1060~C to 1200~C, but very little from 1200~C to 1800~C. Further conclusions must await data for more samples including carbons of many different types and measurements over a larger range of temperature. It is interesting to note that the above data can be -29

-2400 Glassy Carbon/Solid Electrolyte/Graphite -2000 Cgraphite - Cglassy carbon -1800-1200-800 -400- / ~650 75850 950 1050 aSi^ fTEMP ~C 400:K 1200 321-13-10624C ~ Cooling AH =9,029Cal/mole * Heating AS =8.66 Cal/mole-~K ~1200 3 21-3 43CoCooling AH =4,934 Cal/mole 321 - 1:3 -I 243 ~C aHeating AS =4.70 Cal/mole- OK a Cooling AH =3,689 Cal/mole 321-13-18 C A Heating AS =4.60Cal/mole-OK Figure 9. -30

10,000 C -tC 0Graphite 0Glassy Carbon 8000 - 6000 \ 0.0 E ~5 n AH < 4000- 8.0 (n 2000 AS 6.0 0 -1 4.0 1000 1200 1400 1600 1800 2000 Figure 10. HTT (~C) -31

used to directly calculate the ratio of carbon sites occupied by 0 to those free, if one uses data available for reaction 3 and for the oxygen exchange reaction17, C0 + CO(g) = C02(g) + Cf (5) Example calculations are given below. Glassy Carbon Graphite 321-13(1060~C, Vac) Temperature (Cf 3 f 800~C 0.0128 0.0143 1000~C 0.00458 0.01 It can be seen that the surface of glassy carbon is much better covered with oxygen than is graphite at 1000~C. Work has progressed on a structural model for carbons allowing calculation of the entropy of disorder. At present the results are encouraging but not complete enough for presentation. B. Pore Structure The details of pore structure are being investigated with a variety of techniques, including small angle X-ray scattering, scanning electron microscopy, pycnometry, surface adsorption, and Hg porosimetry. Small Angle X-ray Scattering Microporosity is one of the main characteristics of the non-graphitizing carbons. The small angle X-ray scattering -32

permits the evaluation of general structural parameters if recent developments in theory are used to analyze the scattering. Perret and Ruland's18 work on the non-graphitizing carbons gives an outstanding example. The determination of the pore size and the pore size distribution can be made using Guinier's analysis which has been performed on several samples. For the evaluation of RG, the Guinier radius, the approximation I(S) = n2 exp(- 4 T2 RG s2) is considered to be valid. Here I(s) is the observed X-ray intensity and s is 2 sin6/X, where e and X are the Bragg angle and wave length, respectively. The RG can be obtained from a plot of I(s) versus s2, which is a straight line if the distribution of particle size is narrow. Pore size can be calculated from RG if the shape of the pores is known. If the pores are spherical then a= / a 3 RG where a is the radius of the pore. The extent to which the log I(s) versus s2 plot follows a straight line gives information about the pore size distribution. In the case of a wide distribution of pore size, the slope of the I(s) versus s2 curve varies from point to point. Experimental Procedure Copper Ka radiation was employed with pinhole collimation. The intensity was collected on the photographic films. The -33

density of the films was measured using a Joyce-Loebl microdensitometer. The samples in all the cases were a few millimeters thick. Results Figs. 11 and 12 show results for some of the samples studied. As can be seen, most of the samples follow Guinier's law, i.e., the log I versus s2 plot is a straight line. Table 4 gives our values of "a" along with the reported values for some commercial samples. The agreement is not very good. As in our case, the values are almost twice the reported values. However, all three samples follow Guinier's law fairly o well up to S2 = 2 x 10-4A-2 and very little polydispersity is seen which agrees very well with reported results. Table 5 shows the "a" values for some of our samples. It has been found that samples 317-45(2000), 318-11(2000), 318-42 (2000) are not monodisperse. In these cases the pore size has been determined from the average value of the slope. The pore size is smaller for the samples heat treated at 700~C than the samples heat treated at 2000~C. This is in agreement with the work of Perret and Ruland on the non-graphitizing carbons.18 There seems to be a strong correlation between the appearance of multiple reflections in the (002) line and the appearance of polydispersity in small angle scattering. A further investigation of this point is in order. Currently, the unit is being adjusted for the slit colli-34

8 o0 LMSC-2000 x GC-10 * GC-20 4 0 318-48(700) 0 32\X 0~ O \o 0 2 3 4 0 1 2 3 4 S xO4 [A2] Figure 11. Guinier plots for four different samples. Intensity values are in arbitrary units. -35

8 * 318-44(2000) o 318-45(700) x 317-45 (2000) 40 \\ h-J 0 I 2 3 4 012-4 S2 x 104[-2] Figure 12. Guinier plots for three different samples. Intensity values are in arbitrary units. -36

mation so that a counter can be used to determine the intensity and reduce the experimental time per sample. Electron Scanning Microscopy Electron scanning microscopy is employed on a fracture surface of each sample to obtain additional information on the 0 pore structure. For the coarser materials (>200A) the pore structure is easily discernible with this method. However, for the finer materials, the size of the pores is equal to or finer 0 than the 100A resolving power of the instrument, rendering the determination of quantitative information impossible. Also, the SEM pictures show a surface roughness of the same order of size as the pore structure which makes pore size assessment difficult. In many instances, it has been possible to compare the average pore size as measured with SEM to that obtained for Hg porosimetry. The agreement is satisfactory though not precise. For the finer pored materials, lack of resolving power and surface roughness preclude even a rough quantitative check. However, from the observations made on coarser materials, it may be concluded that the Hg intrusion pore diameter is approximately the same as actually seen in the microscope. The microstructures examined show the same general features as presented previously1'2, although some improvement in presence of foreign "agglomerate" particles has apparently resulted from filtering the starting resin. -37

Pycnometry As a routine characterization of the pore volume open to He, the real density was measured in a commercial pycnometer made by Micrometrics Inc. of Norcross, Georgia. Powder samples, -325 mesh, are used routinely. Data for samples thus far measured is included in Table 8. Considerable difficulty has been encountered in the He density measurements for carbons with HTT in the range of 700~C. In this range the carbons are known to have a very large micropore volume which has been verified by our surface area determinations. Data for some of these samples yielded an apparent negative density, probably due to a rather large absorption of He in the micropores of the carbon. While in these cases it is obvious that an error exists, it may be that much of the variation in He density of other samples is caused by smaller, but variable, amounts of adsorption.19 Many of the 700~C samples, however, behaved normally. In general, as expected with these samples, the 700~C density was higher than that at 2000~C as can be seen for example in Table 6. As a result, densities are now being measured by Xylene immersion. In most cases the Xylene density is quite reproducible, and in most cases, slightly lower than the He density as expected. In addition to real density, the apparent density of the bulk samples is determined geometrically. Table 2 includes the results obtained to date. -38

Surface Area Additional surface area data for samples 321-9 have been gathered since those in Table 6 reported previously2. The high surface area (%500 m2/gm) of glassy carbons treated to 700~C was again confirmed, as was the dramatic drop after pyrolysis to 2000~C. Sample 321-9 is characterized by relatively high apparent density and very fine pore size as seen in the Hg porosimetry data of Table 7. However, the open porosity of 0 57 to 73A can not be the porosity accounting for the very high surface area of the 700~C sample as can be seen by comparing the Hg data for the 700~C and 2000~C samples. While the open pore system is about the same size, the 700~C sample has slightly less intrusion pore volume, but almost 50 times the open area for nitrogen adsorption. Similarly, for sample 318-22, the slightly higher Hg intrusion pore volume gives no significantly larger nitrogen surface area. The large surface area is probably assoco 0 iated with the smaller pore system (5-20A) disclosed by small angle scattering and molecular probe techniques. Mercury Porosimetry Mercury porosimetry was used to determine pore size distribution, interconnected pore volume, density and median pore diameter values. Data obtained to date are shown in Table 7. In most cases, a rather sharp pore size distribution was observed, however, a few samples yielded a wide distribution. The porosimetry data indicate that it is possible to produce material with a rather large open pore volume (up to 65%) with a pore size -39

ranging from 30 Angstroms to 50 microns. In addition, there is 0 a pore structure at a smaller level of 5-15A which is open in low temperature carbons to the macropore system. This allows rather exciting possibilities in providing structurally strong, inert elements that could serve both as filters and absorbers. Higher processing temperature (HTT) closes the very fine pores and causes them to grow according to surface area and X-ray scattering results. The macropore system, even though it 0 is very fine (%30A) in some cases, changes relatively little up to 2000~C. In most cases, noted in Table 7, the pore size decreases slightly while the pore volume remains about constant. IV. Property Evaluation Because the glassy carbons under investigation were produced under a wide range of processing variables, a large degree of variation in structure and physical properties was observed. Based on previous information, some of which was included in a previous report2, several tests were chosen as a means of obtaining preliminary mechanical property data. The mechanical properties investigated thus far include hardness (DPH), compressive strength, ultimate tensile strength (Dimetral compression) and sonic modulus of elasticity. In addition, internal friction and electrical resistiveity were measured on selected samples. -40

Hardness Hardness measurements of these materials have posed constant problems, despite the appeal of providing a quick mechanical measurement. At present no test has been found completely satisfactory since the various carbons vary so widely in pore volume and pore size. The indentation in many of the materials occurs largely by densification under the indentor. In most cases there is a large recovery. Attempts were made during this report period to develop a Rockwell type test which measures depth of indentation instead of indentation stress. Satisfactory testing could be done without cracking at rather large loads using a 1/8" diameter ball. However, the results on widely differing carbons failed to correlate with strength, Vickers hardness, modulus, or scratch hardness. Further hardness testing awaits development of a more relevant test. Compressive and Ultimate Tensile Strength Further results are reported in Table 8 and presented on "reduced" basis in Table 9. Values were revised where additional data warranted change. To show the relevance of the diametral disc rupture test, tensile bars 2 inches long by 3/8 inch diameter were ground, threaded gripping ends epoxied in place, and tested in uniaxial tension on an Instron. In this way, a large sample volume is under stress. The results are given in Table 10 showing a very gratifying agreement. The tensile data surpassed the disc results in half the cases. A similar comparison is planned with -41

three point bending tests on very small samples, which normally gives unrealistically high values. The tensile disc test often gives a stepped stress-strain curve which raised the possibility that the pores may be functioning as crack stoppers. This observation can not be definitely confirmed at this time since there is a possibility of compressive failure occurring at the disc edges due to stress concentration before the tensile strength has been exceeded in the center of the sample. However, Tingey has notedll definite acoustic emissions from these materials prior to catastrophic fracture indicating that the steps may indeed correspond to cracking between pores. Various correlations have been attempted between strength properties and processing variables, apparent density, real density and pore size without great success. The raw data show a broad correlation with apparent density; with higher strength occurring at higher density. Also, a fair correlation (Figs. 13 and 14) exists with intrusion pore diameter, higher strengths with smaller pores. No other correlations are evident -at this time. Since strength is controlled by fracture path, it would be determined by the maximum path within the carbon, i.e., distance between pores. For similar structures and constant densities (real and apparent), the mean free path would vary directly with the average pore size. Unfortunately, these conditions are not met between different samples and further, the only measure of the pore size over an adequate range is the mean -42

JO 1 — iiiii i i - ---...... 00 Log Median Pore Diameter vs \ Compressive Strength I ~0 j1 20 60 w 40 0. 0 I L ~ ~ ~ 0O0.01 0 10 20 30 40 50 60 70 COMPRESSIVE STRENGTH PSI x 1000 Figure 13. -43

100 -00[\ ~Log Median Pore Diameter vs X Ultimate Strength 10 0 X w 0 1 \ x\ I \ \ LlI \ I l \ 5 \ x'X 0 2 4 6 8 10 12 14 ULTIMATE STRENGTH PSI x 1000 Figure 14. -4 4-44

intrustion pore size. Attempts to use SEM measurements are not very fruitful since the interesting range occurs at sizes where the path length is not easily measured. The reduced data shown in Table 9 show less range than the raw data. As one method of data reduction, the various mechanical properties are divided by density to yield value of specific strength. On a specific basis these carbon materials compare very favorably with the best available structural materials. Considering the high temperature capability of carbon, the comparison becomes even more favorable. In addition, the area dependent properties have been normalized by either multiplying or dividing by the area fraction carbon, which is proportional to the volume fraction unavailable to He (i.e., Pa/PHe), assuming all pores open to He. It can be seen that this normalization considerably reduces the range of values exhibited by the various carbons. However, since the compressive and tensile strengths are certainly dependent on macrostructure as well as fine scale binding of carbon atoms, some range of reduced properties is to be expected. Sonic Modulus and Internal Friction A conversion factor error was noted in the modulus data presented in the last report2. All data subject to this error have been recalculated reducing the previous results by a factor of.75. However, the extremely wide range possible in porous glassy carbons is still present, i.e., from.35x106 psi to 5.8x106 psi. When the data are reduced to reflect the volume -45

fraction carbon, the range goes from.32x106 psi to 10.06x106 psi, with most samples falling around 2.5x106 psi. This value is reasonably close to that reported for other more dense glassy carbons. However, the existence of such a wide range is quite interesting since the modulus should not be very dependent upon gross microstructure, but should be determined by shorter range carbon-carbon bonding. In order to determine whether the sonic modulus, which involves very small strains, well approximates the mechanical modulus, test bars were fitted with strain gages. Prior calculation had already justified that the difference between adiabatic and isothermal moduli for these materials should be negligible. Table 11 shows a comparison of results, which indeed shows that the sonic modulus is a good measure of the modulus at higher strains. The modulus data versus HTT are shown in Table 12. In all samples the modulus rises from about 104 psi after low temperature curing to about 106 psi after 700~C HTT and then passes through a broad maximum (X3x106 psi) between 900-1500~C HTT. The HTT for this maximum for a single sample series will be investigated including some temperatures below 700~C. The rather remarkable increase in modulus between the cured and pyrolyzed states illustrated below warrants further study. The evolution of the stiffness with curing may be useful in sensing changein n "crosslinking" in a given sample and between -46

samples if a suitable method can be devised for normalizing the data with respect to structural changes. Sonic Modulus, psi Sample Treatment Temperature ~C Sample 70~C 95~C 700~C 318-35 -- 1.52x104.76x106 318-36 -- 2.47xl04 1.2x106 318-37 -- 1.56x104.69x106 318-39.74x10 4 _.9x106 318-45 5.5x104 -- 1.09x106 318-46 6.2x104 --.89x106 Internal friction measurements have been discontinued for the present. While remarkable differences in behavior of the various samples have been noted, no straightforward method of correlating these changes to structure has been developed. The anomalous decay curves found in some samples earlier2 are believed to be associated with mixed frequency excitation due to the specimen claiming device rather than related to porosity as first thought. Resistivity Refinements of the measuring set-up have allowed more accurate measurements, particularly at low resistivity. Cumulative data is presented in Table 13. Resistivity will be continued on a limited basis, especially as a parallel check of sonic modulus data for the low temperature development of crosslinking. It is interesting to note that the resistivity of -47

nearly all samples on a reduced basis falls between 10-3-10-4 Q-cm which is the same as for other glassy carbon materials pyrolyzed to 2000~C. -48

REFERENCES 1. E. E. Hucke, "Glassy Carbons," Semi-Annual Report, January 1972, Contract No. DAHC15-71-C-0283. 2. Ibid, June 1972. 3. C. R. Houska and B. E. Warren, J. Appl. Phys. 25, (1954). 4. D. Kay, Techniquea od Efecaton Miac&ocopy, Blackwell Scientific Publications, Oxford Press, 1967. 5. B. K. Vainshtein, S-tuctute Anatyzis by Etectton Di4daction, MacMillan, New York, 1964. 6. A. G. Whittaker and P. L. Kinter, Science 165, 589 (1969). 7. A. G. Whittaker and B. L. Tooper, "Single Crystal Diffraction Patterns from Vitreous Carbon," to be published. 8. E. E. Hucke and S. K. Das, "A Proposed Method for the Evaluation of the Thermodynamic Properties of the Glassy CarbonGraphite Equilibrium," Preliminary Reports, Memoranda and Technical Notes of the ARPA Materials Summer Conference, July 1971, Contract No. DAHC15-71-C-0253. 9. Y. Takahashi and E. F. Westrum, Jr., J. Chem. Thermo. 2, 847 (1970). 10. J. Yokoyama, M. Murabayashi, Y. Takahashi, T. Mukaibo, Tanso 65, 44 (1971). (Translated from Japanese.) 11. G. L. Tingey, Semi-Annual Technical Report for the Period 2 Nov 71 to 1 May 72, "Investigation of the Influence of Structure on Chemical Stability and Thermal Mechanical Shock Properties of Glass-Like Carbon," Battelle-Northwest Labs., Richland, Washington, June 1972. 12. M. C. Shen and A. Eisenberg, Rubber Chemistry and Technology 43, 95 (1970). 13. J. B. Lewis, R. Murdock and A. N. Moul, Nature 221, 1137 (1969). 14. H. P. Boehm and R. W. Coughlin, Carbon 2, 1 (1964). 15. A. R. Gordon, J. Chem. Phys. 1, 308 (1933). 16. G. L. Hawkes and D. R. Morris, Trans. TMS-AIME 242, 1083 (1968). -49

17. S. Ergun and M. Mentser, Chemi4tty and Physics od Catbon, Vol. 1, p. 203, Marcel Dekker, Inc., New York, 1965. 18. R. Perret and W. Ruland, J. Appl. Cryst. 1, 308 (1968). 19. K. A. Kini and W. O. Stacy, Carbon 1, 17-24 (1963). -50

APPENDIX -151

TABLE 1 SUMMARY OF X-RAY DATA (All values in Angstroms) Symbols Used in the Tables Experimental Condition All the samples were run in a Phillips-Norelco Diffractometer using CuKa radiation under the following conditions: Tube Voltage: 45KV Tube Current: 14mA Proportional Counter Voltage: 1.622KV Proportional Counter Time Constant: 4 sec. Chart Speed: 1/2 inch/min. Scan Speed: 1.2 degree (20)/min. Slits: 1~/006"/1~ at Primary/Scattering/Secondary Sample used of thickness of 3mm in all cases except where otherwise designated. The value of d(10) refers to the unresolved (100) and (101) peak. (002) Peak Type S: "Smooth" (or single phase) Peak NVS: "Not Very Smooth" Peak 2P: "2 Phase" Peak 3P: "3 Phase" Peak (002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La Graphite, solid S 3.37 Very 2.13 Very 3mm & lmm thick High High Graphite S 3.37 Very 2.13 Very High High Graphite, natural S 3.35 Very 2.13 Very (Reported) High High Graphite, synthetic S 3.37 Very 2.13 Very (Reported) High High -52

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La Commercial Samples Lockheed, solid 2000 S 3.53 21.2 2.09 98.0 Lockheed, reported 2000 3.56 19.0 - Beckwith, solid 2000 S 3.55 23.2 2.09 112.0 Beckwith, reported 2000 3.54 15.0 -- 50.0 Tokai, solid 1000 S 3.70 14.2 2.07 43.7 Tokai, reported 2000 -- -- -- Atomergic Chemicals 2500 S 3.52 30.2 2.09 66.0 Co., V-25, solid Atomergic Chemicals 2500 Co., V-25, reported Atomergic Chemicals 1000 NVS 3.44 45.0 2.10 70.0 Co., V-10 Atomergic Chemicals 1000 - Co., V-10, reported 311-9 2000 S 3.54 28.0 2.10 57.0 311-19 700 S 3.63 18.0 -- -- 311-20 2000 S 3.53 27.2 2.10 46.0 311-21 2000 S 3.52 27.2 2.10 54.0 311-22 2000 2P 2.49 29.0 2.12 >125.0 3.45 311-25 700 S 3.70 21.0 -- -- 311-30A 2000 S 3.51 23.4 2.10 54.0 311-31 2000 S 3.50 25.0 2.10 51.0 312-8 2000 S 3.52 27.0 2.10 42.0 312-9 2000 2P 3.52 27.0 2.10 57.0 3.45 312-10 700 S 3.65 16.2 -- -- 312-10 2000 S 3.49 35.0 2.11 53.0 312-14 2000 S 3.51 29.0 2.09 61.0 312-14A 2000 3P 3.46 32.0 2.12 >150.0 3.43 3.36 312-15 2000 S 3.52 27.1 2.11 51.0 312-16 2000 3P 3.47 32.1 2.11 51.0 3.43 3.36 312-21 2000 S 3.51 30.8 2.10 57.0 312-26 2000 S 3.51 27.8 2.09 48.0 312-28 2000 S 3.51 27.2 2.10 51.0 312-29 2000 S 3.51 34.0 2.10 57.0 312-31, solid 2000 S 3.57 27.6 2.10 56.0 312-32 2000 S 3.51 30.8 2.10 54.0 312-33 2000 NVS 3.48 30.8 2.10 52.8 -53

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 312-34 2000 2P 3.46 33.0 2.11 46.2 3.44 312-39 2000 S 3.49 29.8 2.10 53.0 312-40 2000 2P 3.48 30.1 2.09 54.0 3.45 312-43 2000 2P 3.48 33.2 2.11 51.0 3.43 312-44 2000 2P 3.48 42.0 2.11 51.0 3.44 312-48 2000 3P 3.46 30.4 2.10 37.0 3.43 3.37 312-49 2000 S 3.52 31.1 2.11 61.0 315-1 2000 S 3.53 27.2 2.10 48.0 315-2 2000 2P 3.49 29.0 2.10 54.0 3.43 315-3 700 S 3.71 16.2 - 315-5 2000 2P 3.49 29.0 2.11 54.0 3.44 315-8 2000 2P 3.49 28.2 2.10 56.0 3.44 315-9 2000 2P 3.47 33.0 2.11 47.0 3.44 315-14 2000 S 3.53 26.3 2.10 54.0 315-18 2000 3P 3.40 45.0 3.382 3.351 315-20 680 S 3.70 16.3 - 315-20A 2000 2P 3.53 28.0 2.10 57.0 3.43 315-21C 2000 2P 3.52 27.8 2.10 57.0 3.43 315-22 665 S 3.67 16.4 -- -- 315-22 2000 S 3.52 28.0 2.10 51.0 315-24A 2000 2P 3.47 20.0 - 3.38 315-25A 2000 S 3.52 26.5 2.09 48.0 315-26B 2000 3P 3.50 26.5 2.10 46.0 3.41 3.37 315-26C 680 S 3.69 17.1 -- -- 315-28 2000 2P 3.52 26.0 2.10 46.0 3.43 315-28B 600 S 3.70 16.8 -- -- 315-30 2000 2P 3.56 24.0 2.09 48.0 3.43 315-31 680 S 3.70 18.2 -- -- 315-34 680 S 3.69 15.4 -- -- -54

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 315-36 2000 3P 3.52 24.3 2.10 48.5 3.43 3.37 315-37 680 S 3.63 17.5 315-37 2000 S 3.50 26.3 2.098 42.0 315-38 680 S 3.63 18.8 315-38 2000 2P 3.49 27.1 2.097 46.0 3.43 315-39 2000 2P 3.53 27.2 2.098 57.0 3.43 315-39 680 S 3.63 20.0 -- 315-40 2000 S 3.54 25.6 2.097 51.0 315-41 2000 NVS 3.49 23.6 2.098 51.0 315-42 2000 S 3.56 27.2 2.098 46.0 315-43 2000 NVS 3.52 24.3 2.098 51.0 315-43 700 S 3.67 17.4 315-44 2000 2P 3.55 23.1 2.10 40.2 3.45 315-45 2000 S 3.49 27.2 2.10 46.6 315-46A 2000 2P 3.55 23.1 2.098 57.0 3.43 316-6 2000 NVS 3.50 27.0 2.11 57.0 316-7, Run 1 2000 S 3.49 28.0 2.10 45.0 316-7, Run 2 2000 S 3.52 27.0 2.10 53.0 316-15 2000 2P 3.40 32.0 316-28 2000 S 3.50 27.2 2.10 51.0 316-32 2000 2P 3.42 53.0 3.40 317-1 700 S 3.71 20.0 317-1 2000 S 3.46 45.0 2.11 63.0 317-2 700 S 3.68 15.7 317-2 2000 NVS 3.48 24.6 2.09 47.0 317-6 700 S 3.71 13.0 317-6 2000 NVS 3.55 22.0 2.10 55.0 317-7 700 S 3.68 16.0 317-7 2000 NVS 3.46 27.5 2.10 50.0 317-8 700 S 3.71 11.5 317-8 2000 2P 3.56 20.0 2.10 44.0 3.46 317-10 2000 NVS 3.48 26.0 2.10 68.0 317-11 700 S 3.71 16.3 317-13 700 S 3.72 15.0 317-13 2000 NVS 3.47 24.0 2.08 66.0 317-14 700 S 3.71 15.7 317-14 2000 NVS 3.45 27.0 2.09 46.0 317-15 700 S 3.71 15.3 -- -- 317-15 2000 NVS 3.47 26.0 2.09 54.0 317-16 2000 S 3.54 24.0 2.09 53.0 -55

(002) Temp. Peak Sample Designation (oC) Type d(002) Lc d(10) La 317-18 2000 S 3.59 21.0 2.09 58.0 317-19 700 S 3.68 16.5 -- -- 317-19 2000 NVS 3.49 30.0 2.09 52.0 317-20 700 S 3.66 17.5 -- -- 317-20 2000 S 3.50 25.6 2.09 48.0 317-24, Run 1 2000 NVS 3.52 24.0 2.09 45.0 317-24, Run 2, solid 2000 NVS 3.49 21.0 2.09 50.0 317-25 2000 S 3.53 20.0 2.09 50.0 317-26, Run 1 2000 NVS 3.48 26.0 2.09 48.0 317-26, Run 2, solid 2000 2P 3.46 24.2 2.10 51.0 3.43 317-28 2000 NVS 3.46 25.0 2.09 52.0 317-29 700 2P 3.43 21.5 -- -- 3.42 317-29, Run 1 2000 NVS 3.43 65.0 317-29, Run 2 2000 NVS 3.426 75.0 317-30 2000 2P 3.44 29.5 -- -- 3.40 317-31A 2000 S 3.58 22.0 2.10 46.0 317-32 700 S - - 317-32 2000 2P 3.51 23.6 2.08 49.0 3.48 317-33 700 S 3.68 17.0 -- -- 317-33 2000 S 3.414 92.0 2.10 49.0 317-34 700 S 3.68 17.0 -- -- 317-34 2000 3P 3.44 30.0 2.09 50.0 3.42 3.36 317-35 700 S 3.71 16.0 -- -- 317-35 2000 3P 3.50 26.5 2.10 62.0 3.43 3.36 317-37 700 S 3.68 15.6 - 317-37 2000 NVS 3.43 43.0 2.10 63.0 317-38 700 S 3.68 15.6 -- -- 317-38 2000 3P 3.54 25.0 2.09 51.0 3.43 3.37 317-39, Run 1 2000 3P 3.45 28.0 2.10 52.0 3.43 3.36 317-39, Run 2, 2000 3P 3.52 24.2 2.09 45.0 solid, lmm thick 3.42 3.37 317-39, Run 3, 2000 3P 3.52 23.5 2.09 49.0 solid, Imm thick 3.41 3.37 -56

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 317-40 2000 3P 3.49 24.8 2.10 48.0 3.42 3.36 317-41A 2000 S 3.53 26.5 2.10 48.0 317-413 2000 S 3.53 28.0 2.10 54.0 317-42 2000 3P 3.49 26.0 2.10 42.6 3.42 3.36 317-43 2000 3P 3.45 26.0 2.09 56.0 3.42 3.35 317-44 2000 3P 3.48 30.0 2.09 55.0 3.42 3.36 317-45, solid, 700 S 3.75 12.9 -- -- Imm thick 317-45, Run 1 2000 3P 3.48 25.0 2.09 60.0 3.40 3.35 317-45, Run 2 2000 3P 3.46 24.0 2.09 42.0 3.42 3.35 317-46 2000 3P 3.43 31.5 2.10 75.0 3.42 3.36 317-47 2000 3P 3.50 27.0 2.10 60.0 3.42 3.36 317-48, Run 1 700 S 3.71 16.2 317-48, Run 2 700 S 3.87 17.4 317-48, Run 1 2000 3P 3.45 40.0 2.10 60.0 3.43 3.37 317-48, Run 2 2000 3P 3.46 34.0 2.10 59.0 solid, lmm thick 3.43 3.37 317-49 700 S 3.71 15.7 -- -- 317-49, Run 1 2000 3P 3.49 29.0 2.09 62.0 3.41 3.35 317-49, Run 2 2000 3P 3.46 33.0 2.09 60.0 solid, lmm thick 3.44 3.37 317-50 700 S 3.67 15.6 -- -- 318-1 2000 S 3.55 28.0 2.10 54.0 318-2 2000 S 3.51 27.0 2.10 55.0 318-3, Run 1 700 S 3.70 16.7 -- -- 318-3, Run 2 700 S 3.69 16.7 -- -- -57

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 318-3 2000 2P 3.46 26.0 2.11 51.0 3.41 318-4 700 S 3.66 16.8 - 318-6A 2000 S 3.50 31.0 2.09 59.0 318-7, Run 1 2000 S 3.50 28.0 2.10 65.0 318-7, Run 2, solid 2000 S 3.49 28.0 2.10 45.0 318-8, Run 1 2000 S 3.45 39.0 2.10 63.0 318-8, Run 2 2000 S 3.45 43.5 2.10 77.0 solid, 2mm thick 318-9 2000 2P 3.48 32.5 2.11 57.0 3.46 318-10 520 S 3.74 15.2 -- -- 318-10 2000 S 3.49 33.8 2.12 50.0 318-11, Run 1 2000 NVS 3.42 77.0 2.10 38.0 318-11, Run 2 2000 NVS 3.43 78.0 2.11 40.0 318-12 2000 3P 3.49 31.4 2.09 59.0 3.43 3.36 318-13 2000 NVS 3.42 44.0 2.10 58.0 318-14 700 S 3.65 16.0 -- -- 318-14 2000 3P 3.48 30.5 2.10 60.0 3.43 3.36 318-15, Run 1 700 S 3.75 16.0 -- -- 318-15, Run 2 700 S 3.75 15.1 -- -- 318-15 2000 3P 3.45 30.2 2.10 60.0 3.42 3.37 318-16 700 S 3.72 15.7 -- -- 318-16 2000 2P 3.43 39.0 2.09 49.0 3.41 318-17 700 S 3.68 16.7 -- -- 318-17 2000 NVS 3.45 42.0 2.11 59.0 318-18, Run 1 700 S 3.68 16.4 -- -- 318-18, Run 2 700 S 3.71 16.3 -- -- 318-18 2000 S 3.55 25.6 2.10 44.0 318-19 2000 S 3.52 26.0 2.09 59.0 318-20 700 S 3.67 16.0 -- -- 318-20 2000 S 3.53 21.0 2.09 48.0 318-21, Run 1 700 S 3.78 14.0 -- -- 318-21, Run 2 700 S 3.75 15.4 -- -- 318-21 2000 S 3.55 23.6 2.10 55.0 318-22 700 S 3.70 15.4 -- -- 318-22, Run 1 2000 NVS 3.44 65.0 2.10 55.0 318-22, Run 2 2000 NVS 3.44 64.0 2.11 54.0 318-23 700 S 3.74 16.0 -- -- 318-23 2000 S 3.63 63.0 2.10 73.0 318-24 700 S 3.64 16.7 -- -- -58

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 318-24 2000 S 3.44 45.0 2.10 68.0 318-26, Run 1 700 S 3.69 15.7 - 318-26, Run 2 700 S 3.75 16.1 318-26, Run 3 700 S 3.69 16.7 - 318-27 2000 2P 3.45 35.4 2.10 47.0 3.41 318-28 700 S 3.75 18.0 -- -- 318-28 2000 2P 3.47 27.0 -- -- 3.42 318-29, Run 1 2000 NVS 3.45 30.0 2.08 62.0 318-29, Run 2, 2000 2P 3.50 30.5 2.10 65.0 solid, Imm thick 3.44 318-29, Run 3 2000 2P 3.52 31.0 2.10 60.0 3.42 318-30 700 S 3.64 15.2 -- -- 318-30, Run 1 2000 2P 3.48 34.1 2.11 69.0 3.43 318-30, Run 2 2000 3P 3.45 31.0 2.11 63.0 3.41 3.36 318-31, Run 1 2000 2P 3.45 35.5 2.10 64.0 3.43 318-31, Run 2 2000 3P 3.47 31.0 2.11 63.0 3.41 3.36 318-32, Run 1 700 S 3.64 15.7 318-32, Run 2 700 S 3.63 16.0 - 318-32 2000 S 3.44 47.0 2.10 65.0 318-33 700 S 3.66 16.7 -- -- 318-33 2000 NVS 3.46 28.0 2.11 64.0 318-34 700 S 3.63 16.5 - 318-34 2000 3P 3.49 37.0 2.10 59.0 3.43 3.36 318-35 700 S 3.71 15.3 - 318-35 2000 3P 3.50 34.0 2.11 67.0 3.44 3.37 318-36 700 S 3.68 17.0 -- - 318-36 2000 2P 3.51 28.0 2.10 49.0 3.44 318-37 700 S 3.71 16.1 -- -- 318-37 2000 3P 3.46 33.6 2.10 52.0 3.43 3.376 318-38 700 S 3.71 15.6 -- -- 318-38 2000 3P 3.47 28.0 2.10 49.0 3.43 3.37 -59

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 318-39, Run 1 700 S 3.71 17.0 318-39, Run 2 700 S 3.65 17.2 -- solid, lmm thick 318-39 2000 S 3.51 26.1 2.09 60.0 318-40 700 S 3.71 15.0 - 318-40 2000 2P 3.52 28.0 2.11 54.0 3.45 318-41 700 S 3.71 14.8 -- -- 318-41 2000 S 3.50 28.0 2.09 57.0 318-43, Run 1 700 S 3.69 17.0 -- -- 318-43, Run 2 700 S 3.71 13.8 -- -- solid, lmm thick 318-43, solid 2000 S 3.44 31.0 2.12 58.0 318-44 700 S 3.72 15.6 -- -- 318-44 2000 S 3.55 27.2 2.10 44.0 318-45 700 S 3.71 15.7 -- -- 318-45 2000 S 3.56 25.4 2.10 46.0 318-46 700 S 3.71 15.9 -- -- 318-46, solid 2000 S 3.53 26.2 2.11 51.0 lmm thick 318-47 700 S 3.71 15.0 -- 318-47 2000 NVS 3.49 29.0 2.10 48.0 318-48, Run 1 2000 S 3.53 26.8 2.10 54.0 318-48, Run 2 2000 S 3.52 29.2 2.10 42.0 318-50, Run 1 700 S 3.71 14.3 -- -- 318-50, Run 2 700 S 3.71 15.5 -- -- 318-50 2000 S 3.53 26.0 2.10 46.0 318-51 2000 S 3.56 27.2 2.10 56.0 318-52 2000 S 3.53 26.5 2.10 54.0 318-53, Run 1 2000 S 3.52 26.5 2.10 54.0 318-53, Run 2 2000 S 3.54 30.0 2.10 60.0 318-54 700 S 3.66 17.0 -- -- 318-55 700 S 3.71 15.2 - 318-56 2000 S 3.54 27.0 2.10 54.0 318-58 700 S 3.71 18.0 - 318-58 2000 NVS 3.51 28.2 2.10 51.0 318-59 700 S 3.68 16.7 318-59 2000 S 3.51 26.0 318-60 700 S 3.70 15.7 318-60 2000 2P 3.47 32.0 3.44 318-61 700 S 3.71 18.6 -- -- 318-61 2000 S 3.52 23.3 2.09 55.0 318-62 700 S 3.70 15.3 - 318-62 2000 S 3.56 22.5 2.10 51.0 321-1 700 S 3.66 5.0 -- -- 321-2 700 2P 3.63 17.4 -- -- 3.57 -60

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 321-2 2000 3P 3.54 22.8 2.10 51.5 3.43 3.38 321-3 700 S 3.64 17.4 - 321-3 2000 S 3.53 24.3 2.10 51.0 321-4 700 S 3.64 17.2 -- -- 321-4 2000 - -- -- 321-5 700 S 3.63 15.4 -- -- 321-5 2000 S 3.49 26.4 2.09 53.7 321-6 700 S 3.64 17.0 -- -- 321-6 2000 S 3.54 27.7 2.10 48.0 321-7 700 S 3.69 18.0 -- -- 321-7 2000 - -- -- 321-8 700 S 3.69 17.5 321-8 2000 - -- -- 321-9 700 S 3.67 17.4 321-9 2000 - -- -- 321-10 700 S 3.67 17.0 321-10 2000 - -- -- 321-11 700 S 3.71 17.0 321-11 2000 2P 3.54 27.2 2.10 65.0 3.46 321-12 700 S 3.63 16.8 -- -- 321-12 2000 S 3.53 26.4 2.094 56.0 321-13 700 S 3.66 17.0 -- -- 321-16A 2000 3P 3.50 30.8 2.10 57.0 3.43 3.36 321-16B 2000 S 3.50 28.8 2.10 44.0 321-16C 700 S 3.63 15.2 -- -- 321-17 700 S 3.60 18.7 -- -- 321-17B 2000 S 3.49 28.8 2.10 44.0 321-18A 2000 3P 3.50 29.8 2.10 49.0 3.43 3.37 321-18B 700 S 3.63 15.2 -- -- 321-19A 2000 2P 3.54 25.0 2.09 46.0 3.426 321-19A 700 S 3.63 17.1 -- -- 321-19B 2000 NVS 3.43 39.0 2.10 53.8 321-20A 700 S 3.63 17.5 - 321-20A 2000 3P 3.52 28.0 2.10 61.0 3.42 3.36 321-20B 2000 3P 3.53 37.0 2.10 46.0 3.426 3.37 321-21A 700 S 3.63 18.0 -- -- -61

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 321-21A 2000 NVS 3.43 41.6 2.10 51.0 321-21B 700 S 3.64 18.4 - 321-21B 2000 S 3.52 27.0 2.10 57.0 321-22A 2000 2P 3.52 27.6 2.10 53.0 3.43 321-22B 700 S 3.70 16.1 - 321-23 2000 S 3.49 33.0 2.10 54.0 321-23A 700 S 3.63 18.4 -- -- 321-23B 700 S 3.36 16.5 -- -- 321-23B 2000 3P 3.52 29.6 2.10 51.0 3.43 3.36 321-24 700 S 3.70 15.8 -- -- 321-24A 700 S 3.63 16.2 321-24B 700 S 3.63 16.5 -- -- 321-24B 2000 S 3.43 35.4 2.09 57.0 321-25 700 S 3.63 18.4 -- -- 321-25 2000 NVS 3.47 30.8 2.10 60.8 321-25A 700 S 3.60 21.0 - 321-25A 2000 NVS 3.43 40.2 2.10 60.5 321-26 700 S 3.67 15.0 -- -- 321-26 2000 S 3.52 27.2 2.094 48.5 321-26A 700 S 3.63 18.1 -- -- 321-26A 2000 S 3.52 27.2 2.094 54.0 321-27 2000 S 3.52 29.8 2.10 51.0 321-29 700 S 3.63 16.8 -- -- 321-29 2000 3P 3.49 24.8 2.094 58.0 3.40 3.35 321-30 700 S 3.63 19.6 -- -- 321-31 2300 3P 3.44 49.0 2.10 60.5 3.41 3.37 321-31A 2300 NVS 3.40 90.0 2.11 58.0 321-31B 2300 3P 3.49 37.0 2.11 69.0 3.43 3.37 321-31C 700 S 3.60 18.8 - 321-31C 2300 3P 3.49 34.5 2.11 69.0 3.426 3.37 321-31D 700 S 3.63 17.4 - 321-31D 2300 S 3.47 37.2 2.11 69.0 321-31E 700 S 3.63 17.4 -- -- 321-31E 2300 NVS 3.426 61.6 2.11 69.0 321-31F 700 S 3.60 18.5 - 321-31F 2300 S 3.45 44.0 2.10 69.0 321-31G 2300 2P 3.47 35.0 2.10 56.0 3.43 -62

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 321-311 2300 2P 3.49 40.0 2.11 69.0 3.38 321-32 700 S 3.60 18.9 -- -- 321-34A 2300 S 3.426 51.4 2.10 42.0 321-36A 2300 S 3.47 53.6 2.11 64.5 321-36B 700 S 3.63 18.2 - 321-36C 2300 S 3.43 70.0 2.10 46.0 321-37 2000 S 3.52 30.8 2.10 54.0 321-37A 700 S 3.60 18.1 -- -- 321-37B 2000 3P 3.53 27.2 2.10 54.0 3.44 3.36 321-38B 700 S 3.63 17.7 - 321-39 2000 2P 3.48 34.1 2.10 57.0 3.426 321-39B 700 S 3.63 16.4 -- -- 321-41C 2000 3P 3.49 32.6 2.10 62.5 3.43 3.36 321-42A 700 S 3.63 18.8 -- -- 321-42A 2000 2P 3.49 35.5 2.10 60.5 3.43 321-42B 700 S 3.63 16.7 -- -- 321-42B 2000 2P 3.50 25.3 2.10 64.4 3.43 321-43B 700 S 3.63 19.3 -- -- 321-43B 2000 2P 3.49 35.0 2.098 59.4 3.42 321-43B1 2000 2P 3.50 36.8 2.11 59.5 3.426 321-43B2 2000 2P 3.50 33.0 2.10 57.0 3.43 321-44A 2000 3P 3.50 30.8 2.10 51.0 3.43 3.36 321-44B 2000 3P 3.50 29.0 2.10 54.0 3.43 3.36 321-45A 2200 S 3.49 33.0 2.10 57.0 321-45B 2200 S 3.47 45.5 2.10 40.5 321-46A 2000 2P 3.49 31.7 2.10 60.4 3.43 321-46B 2000 3P 3.46 30.8 2.10 51.0 3.43 3.36 321-46C 2000 3P 3.47 35.6 2.10 51.0 3.43 3.36 -63

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 321-46D 2000 3P 3.50 31.7 2.10 64.4 3.43 3.36 321-48A 2000 S 3.50 31.8 2.10 57.0 321-48B 2000 S 3.50 33.0 2.10 64.4 321-48C 2000 S 3.50 33.0 2.10 60.4 321-49A 2000 S 3.49 33.0 2.10 60.4 321-49B 2000 NVS 3.426 51.2 2.10 54.0 321-51 2000 NVS 3.43 91.5 2.11 69.0 321-51A 2000 NVS 3.43 107.5 2.11 68.0 321-52 2000 NVS 3.43 91.2 2.11 60.5 322-1A 2000 3P 3.44 26.4 2.085 57.3 3.37 3.33 322-1B 2000 S 3.40 41.5 2.085 -- 322-2B 1600 S 3.50 23.0 2.085 37.3 322-3B 1600 S 3.53 22.0 2.085 61.0 322-10A 2000 2P 3.46 33.0 2.085 -- 3.42 322-10B 2000 2P 3.50 30.8 2.10 69.0 3.43 322-10C 2000 2P 3.49 33.4 2.085 -- 3.43 322-10D 2000 2P 3.50 28.6 2.10 60.0 3.43 322-11A 1670 S 3.55 22.0 2.085 51.2 322-12A 1600 S 3.56 23.0 2.085 40.5 322-12B 1670 S 3.56 22.0 2.10 57.0 322-13B 1670 S 3.53 31.8 2.085 50.2 322-14A 1670 S 3.50 23.0 2.085 -- 322-14B 1670 S 3.56 21.0 2.09 46.0 322-15B 1670 S 3.56 25.0 2.085 48.4 322-16A 1670 S 3.56 23.5 2.085 -- 322-16B 1670 S 3.56 22.0 2.085 44.0 322-17A 1670 S 3.56 22.2 2.085 88.0 322-17B 1670 S 3.56 22.0 2.085 51.4 322-18B 1670 S 3.50 28.8 2.085 61.5 322-19B 1670 S 3.56 20.6 2.085 48.5 322-20 1670 S 3.50 21.4 2.085 30.2 322-21B 1670 S 3.56 17.0 2.085 69.5 322-25A 1410 S 3.56 18.5 2.085 46.1 322-25B 1410 S 3.56 19.2 2.07 121.0 322-26A 1410 S 3.50 25.6 2.085 51.0 322-26B 1410 S 3.50 19.2 2.085 40.2 322-27A 1410 S 3.59 20.0 2.085 57.3 322-27B 1410 S 3.56 19.3 2.085 -- 322-28A 1410 S 3.56 19.4 2.08 42.0 322-28B 1410 S 3.56 17.8 2.085 53.2 -64

(002) Temp. Peak Sample Designation (~C) Type d(002) Lc d(10) La 322-29 1410 S 3.56 20.1 2.085 40.2 322-29B 1410 S 3.56 21.0 2.085 53.2 322-31A 1410 S 3.56 23.0 2.085 40.4 322-36 1543 S 3.56 19.2 2.085 53.0 322-37 1543 S 3.56 23.0 2.085 -- 322-40 1440 S 3.53 23.6 2.085 66.0 322-41 1440 S 3.56 20.4 2.085 61.0 322-42A 1440 S 3.56 21.4 2.085 37.1 322-42B 1440 S 3.56 21.4 2.085 65.0 322-46 1440 S 3.53 19.6 2.08 -- 322-47A 1440 S 3.50 21.5 2.085 74.0 -65

TABLE 2 Sizes of the Structural Features Observed in Bright and Dark Field Electron Micrographs Compared to Crystallite Sizes Obtained from X-ray Analysis Granu- Dark Field (002) Platelet latiop* Dia. X** X-ray (i) Peak Sample # Dia. A Dia. A (002) (100) Lc La Type 311-19(2000) 150-500 30-40 20-40 - 311-19(750)X 150-350 20-30 - -- 14 19 S 312-31(2000) 200-500 20-45 20-45 -- 27.6 56 S 312-31(2000) 150 35 30 >100 28 56 S 317-24(2000) 250 42 60t -- 24 45 NVS 317-29(2000) >250 60 30-70t -- 65-75 -- NVS 317-33(2000) 250-500 35 - -- 92 49 S 317-45(2000) >500 30 - -- 25 60 3P 317-48(2000)x 250 55 -- - 34 59 3P 317-49(2000)X 250-500 45 40t -- 33 60 3P 318-12(2000) 250-500 60 50 110t 31 59 3P 318-22(2000) >500 40-60 35 -- 65 55 NVS 318-22(700) 250 -- -- 15.7 -- S 318-23(2000) 250 50 50 -- 63 73 S 318-23(700) -- - - - 16 -- S 318-29(2000)x >500 30-40 60 -- 31 63 2P 321-31C(2000)X 250 35 60 80 35 69 3P 321-31D(2300) 250 40 35 80 37 69 S *Diameter corresponds to distances between nearest neighbor. **Diameter of diffracting regions obtained from (002) or (100) diffraction halos. tSome of the crystallites giving rise to halos or spots are very large in size, i.e., up to 500A. XA second structural feature was observed in the bright field micrographs of these samples. This new feature appeared to be long regular cylinders 500A in diameter by about 1 long. Regular striations along the length were spaced 45A apart. -66

TABLE 3 Electron Diffraction Results Compared to X-ray Diffraction Results for d(002) and d(10) Spacings (A) Electron X-ray Diffraction (002) Sample # d(002) d(10) d(002) d(10) Peak Type Graphite 3.35 2.13 3.37 3.12 311-19(2000) 3.56 2.17 3.45 2.09 311-19(750) 3.70 2.19 -- 2.07 S 312-31(2000) 3.54 2.12 3.53 2.16 S 3.57 2.10 3.53t 2.12 S 317-24(2000) 3.50 2.10 3.53t 2.10t NVS 317-29(2000) 3.43 - 3.35t 2.12 NVS 3.45 317-33(2000) 3.414 2.10 3.35t 2.10 S 317-45(2000) 3.35 2.09 3.50 2.10 3P 3.48 317-48(2000) 3.46 2.10 3.48t 2.12 3P 317-49(2000) 3.48 2.09 3.48t 2.10 3P 318-12(2000) 3.49 2.09 3.47t 2.11 3P 318-22(2000) 3.44 2.10 3.37t 2.07 NVS 318-22(700) 3.70 -- 3.50 2.11 S 3.42t 318-23(2000) 3.43 2.10 3.50t 2.10 S 318-23(700) 3.74 - - 2.07 S 318-29(2000) 3.45 2.08 3.45 2.12 2P 321-31C(2300) 3.43 2.11 3.56t 2.12 3P 321-31D(2300) 3.47 2.11 3.50* 2.125 S *In this sample no spots were seen on any diffraction halo. tIn addition to Debye-Scherrer rings, a number of sharp diffracting spots were observed on or close to the ring. -67

TABLE 4 Sample a in A Dispersity Our value Reported Value LMSC-20 42.4 17.1 Monodisperse GC-10 14.0 9.0 GC-20 12.9 11.5 TABLE 5 Sample a in A Dispersity 312-31 (2000) 40.8 Polydisperse 317-45 (2000) 21.2 Wide distribution of pores 318-11 (2000) 20.4 Bidisperse 44.4 318-41B (700) 18.7 Monodisperse 318-42 (2000) 41.0 Polydisperse 318-44 (2000) 30.4 Monodisperse 318-45 (700) 28.0 Monodisperse 318-45 (2000) 35.3 Monodisperse 318-46 (2000) 20.4 Monodisperse 318-48 (700) 9.5 Monodisperse 318-48 (2000) 25.4 Monodisperse -68

TABLE 6 Surface Area Specific Surface He Density Knudsen Flow Area Sample # Temp. ~C (gm/cm3 (m2/gm) (m2/gm) 311-32 2000 1.41 3.0 26.4 317-9 700 1.83 -- 506.0 317-9 2000 1.70 12.5 59.9 317-12 700 1.80 9.1 510.0 317-12 2000 1.72 -- 109.0 318-22 700 1.79 -- 459.0 318-22 2000 1.51 -- 49.6 321-9 700 1.46 -- 541.2 321-9 2000 1.36 -- 12.7 -69

TABLE 7 PHe real1 PHg real2 PHg app. MPD IPV Sample # Temp.~C (g/cc) (g/cc) (g/cc) () (cc/g) GC No.1 1.47 1.482 1.424.003.0273 302-5 2320 -- 1.509.647 2.97.8828 302-12 2320 -- 1.501.559 3.62 1.1224 305-6 2000 1.94 1.802.636 2.54 1.0151 6.62 Mo 305-12 2000 1.55 1.562.557 4.19 1.1560 305-18 2000 1.77 1.718.606 2.49 1.0678.4 Mo 308P-2 #2 1.586 1.505 1.034.009.3030 308P-3 #3 1.611 1.486 1.077.008.2559 310-1 1000 1.27 1.446.814.023.5411 310-3 1000 -- 1.424.805.020.5454 310-17A 2000 1.50 1.175.639.119.7130 310-18 1000 1.48 1.452.687.039.7666 310-18 2000 1.15 1.366.648.044.8110 310-20 2000 1.09 1.458 1.029.009.2855 310-29 2000 1.89 1.533.944.014.3959 311-21 2000 1.59 1.339.731.038.6221 311-22 2000 1.00.847.484.154.8809 312-19A 730 1.20 1.481.879.629.4626 312-29 728 1.52 1.441 1.038.014.2709 312-31 2000 1.41 1.490.923.025.4118 312-45 2000 1.26 1.302 1.214.005.0540 312-48 2000 1.53 1.392.861.121.4425 312-49 2000 1.34 1.404 1.031.011.2579 315-1 2000 1.50 1.431.962 47.0.3412 317-5 2000 1.42 1.313.873.071.4039 317-18 2000 1.50 1.255.953 39.1.281 318-22 700 1.79 1.426.771.057.5958 318-22 2000 1.51 1.576.937.054.4334 318-45 2000 -- 1.20.78.0078.021 321-9 700 1.46 1.24.98.0073.205 321-9 2000 1.26 1.4 1.2.0057.016 321-17 2000 1.43 1.17.59 2.15.299 321-18 2000 1.67 1.16.87.175.247 321-19 2000 1.80 1.56.98.049.379 321-20 2000 1.60 1.63.70.088.345 321-21 2000 1.79 1.30.85.041.377 321-25 2000 -- 2.20 1.14.011.088 *Glassy Carbon No. 1 - Le Carbone, p. 6927.'Real density as determined by He pycnometry 2Real density as determined by Hg -70

PHe real1 PHg real2 PHg app. MPD IPV Sample # Temp.~C (g/cc) (g/cc) (g/cc) () (cc/g) 321-31 2000 1.41 1.49 1.34.0195.075 322-14A 1300 2.2.826 322-14A 1412 1.74 1.7.494 322-14B 1300 2.3.501 322-14B 1412 1.5.496 322-17A 1300 4.5.604 322-17A 1412 4.4.271 322-17B 1300 2.5.382 322-17B 1412 2.0.534 322-19A 1300 1.0.461 322-19A 1412 1.9.08.472 322-19B 1300.65.466 322-19B 1412.95.468 322-20 1300 1.8.432 322-20 1412 1.5.666 322-21A 1300 18..503 322-21A 1412 3.5.420 322-21B 1412 10..400 322-21D 1300 8..780 322-22A 1300 1.1.308 322-22A 1412 1.2.443 322-22B 1300 1.4.457 322-22B 1412 1.49X* 1.2.440 322-23A 1300 1.5.443 322-23A 1412 1.2.458 322-23B 1300 2.03X.32.453 322-23B 1412.35.458 322-24A 1300 1.74X 1.3.395 322-24A 1412 1.3.563 322-24B 1300 1.9.620 322-24B 1412 1.59X 1.4.888 322-32 1350 1.60X 1.4.571 322-35 1350 1.43X 6.0.472 322-41 1440 1.59X.07.669 322-45 1500 1.72X 4.2.421 322-46 1500 1.4.550 322-47A 1500 1.3.652 322-48 1605 6.0.634 322-49 1400 7.0.841 322-49 1400 7.0.607 322-49 1600 7.0.595 322-50 1600 6.0.545 322-50 1400 6.0.679 *X indicates Xylene -71

TABLE 8 Physical Properties Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. PHe Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xlO) (DPH) (x103) (xlO-6) (x10-3) (x10-3) 310-35 2000 0.57 - -- -- - -- 5.18 1.01 311-34 2000 0.60 -- -- -- -- -- 7.2 7.04 311-35 2000 0.51 --.294 -- 1.43 0.35 6.85 1.23 312-13 2000 1.07 - -- -- -- -- 50.0 4.85 312-14 2000 1.00 1.44 - - -- -- 36.0 - 312-16 2000 0.77 1.27 - -- - -- 1.73 2.83 312-27 2000 1.15 - - - -- -- -- 7.78 312-29 2000 1.07 1.52 - -- - -- 39.7 - 312-32 2000 0.90 1.47 - -- -- - 29.2 5.13 312-33 2000 -- 1.59 -- 90 -- - 312-34 2000 0.92 1.38 -- -- -- - 27.3 1.11 312-44 2000 -- 1.18 -- 98 -- - 312-45 680 -- -- - 135- -- 321-45A 2000 -- 1.26 - 176 312-46 680 - -- -- 107- -- 312-46 2000 -- - - 105- - - 312-49 2000 1.10 1.3 - -- - -- -- 5.96 315-1 2000 0.89 1.49 --- -- -- - 315-2 2000 0.70 1.52.349 -- - 1.27 1.47 0.36 315-3 2000 -- 1.38 --- -- -- - 315-4 2000 -- 1.55 - -- - 315-14 2000 0.96 1.6 -- -- - 47.7 4.7 315-17 2000 0.79 -- - -- - -- 29.3 2.51 315-20 2000 0.84 1.6 --- -- -- - 315-20A 2000 0.84 1.6.180 -- 0.93 1.48 315-20B 2000 0.77 1.60.275 -- 1.63 1.37 315-20C 2000 0.88 1.60.203 -- 0.54 1.52 - 315-21B 2000 0.96 - -- - -- - - 6.60 315-21C 2000 0.91 1.52.147 -- 0.26 1.54 46.8 7.13

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app PHe Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xlO) (DPH) (x103) (x10-6) (x10-3) (x10-3) 315-21D 2000 1.01 - -- - -- -- 2.70 7.62 315-22 2000 0.90 1.63 315-24 2000 1.15 1.78 - - 315-25A 2000 0.88 -- - - -- -- 24.3 4.61 315-25B 2000 0.87 - - -- - - -- 4.78 315-25C 2000 0.88 1.41.317 -- 2.38 1.55 35.5 7.38 315-26B 2000 0.88 - - -- -- - 30.5 6.63 315-26C 2000 0.80 1.45.057 - -- 1.20 25.6 4.24 315-26D 2000 0.83 1.45.149 - -- 1.38 36.6 315-28 2000 0.96 1.46 - - -- - 37.3 4.39 315-30 2000 0.91 1.49 315-31 2000 0.85 1.48 315-31B 2000 0.80 1.46.119 -- 0.33 1.44 35.1 5.15 315-31C 2000 0.93 1.48.237 -- 0.47 1.65 315-31D 2000 0.91 1.46.229 -- 0.42 1.60 36.2 6.6 315-32 2000 0.99 1.43 - -- - -- 45.0 6.35 315-33 2000 0.78 1.50.195 -- 1.50 1.26 315-34C 2000 0.60 1.58.294 -- 0.31 0.87 21.0 2.95 315-34D 2000 0.66 1.57.137 -- 2.01 1.22 16.4 2.73 315-35B 2000 0.87 1.89 315-37 2000 0.53 1.61.262 -- 0.31 0.61 14.2 2.51 315-38 2000 0.72 1.51 315-38A 2000 0.72 1.51.237 - -- 0.93 2.40 2.97 315-39A 2000 0.96 1.64.188 -- 0.47 1.78 35.9 5.59 315-39B 2000 0.96 1.64.029 -- 1.28 1.76 28.5 4.41 315-40 2000 0.87 1.33 315-41 2000 0.68 1.67.220 - -- -- 15.0 315-41A 2000 0.77 1.67.038 -- 1.18 1.35 18.6 2.0 315-41B 2000 0.79 1.67.157 - 0.98 1.28 16.0 2.02 315-42 2000 0.87 1.83.249 -- 0.35 1.65 315-43 2000 1.04 1.90 -- - - -- 50.0 -- 315-44 2000 0.76 1.78.214 -- 0.32 1.43 315-45 2000 0.88 1.66 -

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. PHe Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xlO) (DPH) (x103) (x10-6) (x10-3) x10-3) 315-45B 2000 0.76 1.39.039 -- 0.28 5.8 315-46 2000 1.094 -- -- 240 - -- - 315-46 2000 1.094 -- - 105 --- 315-46A 2000 0.899 1.55 -- 58 -- - 2.5 2.23 317-1 2000 1.21 1.67 - -- -- -- 56.5 7.5 317-2 2000 0.71 1.74.088 -- - 0.91 23.7 2.97 317-5 2000 0.78 1.42 -- 58 - -- 33.1 7.50 317-6 2000 0.78 1.88 --- --- 317-7 2000 0.79 1.82 -- --- 317-8 2000 0.90 1.64 -- -- - 1.82 40.5 2.29 317-9 2000 0.93 1.76 - - -- -- 32.3 5.77 317-10 2000 0.79 1.42.009 -- 0.75 1.45 43.7 6.00 317-12 2000 0.89 1.60 - - -- -- - 5.82 317-13 2000 0.88 1.88- - --- 317-14 2000 0.87 1.49 - -- - -- 27.4 4.69 317-15 2000 0.91 1.46 - - -- - 33.6 4.09 317-18 2000 0.72 1.50.088 -- 0.39 0.86 5.1 3.30 317-19 2000 1.13 1.68 - - -- -- 28.2 8.75 317-20 2000 1.05 1.51- -- --- 317-23 2000 0.83 -- -- -- -- 7.6 1.90 317-24 2000 0.76 1.57.187 -- 0.76 1.45 49.1 4.37 317-25 2000 0.88 1.69 -- -- -- - 34.1 2.85 317-26 2000 0.78 1.48.195 14 0.66 1.51 4.7 0.92 317-27 2000 -- -- -- -- - - 37.3 - 317-28 2000 0.93 1.7 --- -- --- 317-29 2000 0.74 1.65.122 - -- 0.86 16.4 2.48 317-30 2000 0.77 1.68 --- -- --- 317-31 2000 0.70 1.45 --- -- --- 317-32 2000 0.89 1.72.224 -- - 1.64 44.2 5.05 317-33 2000 1.02 1.46 -- 73 - -- 40.2 5.60 317-34 2000 0.65 1.56.321 -- - 2.07 24.0 4.61 317-35 2000 0.98 1.40 - -- -- - --- 317-37 2000 0.90 1.34.225 80 0.31 1.61 40.6 6.90

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app.- He Resistivity ness Frict. psi psi psi Sample # Temp.C (g/cc) (g/cc) Q-cm(xlO) (DPH) (x103) (x10-6) (x10-3) (xl-3) 317-38 2000 0.92 1.34.268 62 1.27 1.01 37.6 4.20 317-39 2000 0.77 1.27.032 49 0.19 1.20 26.7 3.58 317-40 2000 0.86 1.47.184 -- -- 1.25 22.8 3.44 317-41 2000 0.93 - - - - -- 10.0 2.35 317-41A 2000 0.90 -- - - -- -- 7.4 1.91 317-41B 2000 1.12 1.48 -- -- -- -- 27.0 3.90 317-42 2000 0.87 1.45.135 53 - 1.54 39.8 5.30 317-43 2000 0.90 1.40 -- -- -- -- 15.0 2.47 317-44 2000 0.84 1.51.007 52 1.68 1.35 27.3 2.13 317-45 2000 0.88 1.40 -- -- -- -- 32.3 5.2 317-46 2000 0.81 1.48.112 71 - 1.27 34.6 4.95 317-47 2000 0.97 1.39 -- 49 -- - 27.5 5.62 317-48 2000 1.16 1.46 -- -- -- 1.23 -- 317-49 2000 0.80 1.51.34 - 1.31 0.89 11.1 3.0 318-1 2000 0.79 1.51.169 -- -- 0.71 -- 2.56 318-2 2000 0.95 1.45 -- -- -- 318-2C 680 0.89 -- 907.0 - - 0.80 34.5 4.77 318-3 2000 -- 1.37 -- -- -- 318-6A 2000 1.17 1.45 -- -- -- 318-7 2000 0.78 --.165 - - 0.65 0.82 1.67 318-8 2000 0.96 1.49 -- 60 - - 18.2 5.62 318-8A 2000 0.97 -- - -- - - 32.7 318-9 2000 0.96 1.50 - 56 - - 27.4 5.19 318-10 2000 0.99 1.48 -- 318-11 2000 0.91 1.58 - 51 - 1.48 - 5.09 318-12 2000 0.98 1.50 - 61 -- 318-13 2000 1.03 -- -- 71 -- -- -- 318-14 2000 0.77 1.47.285 31 0.41 0.41 4.74 0.83 318-15 2000 0.95 1.51 -- 40 -- 318-16 2000 0.94 1.48.270 47 - 1.43 28.2 4.02 318-17 2000 0.74 1.46.189 53 0.18 1.18 33.2 4.35 318-18 2000 -- 1.48 -- 46 -- -- -- 318-18B 2000- -- -- -- - - - 5.28

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. PHe Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xlO) (DPH) (x103) x10-6) x10-3) x10-3) 318-19 2000 0.77 1.41 -- --- 318-20 2000 -- 1.50 -- 65- -- 318-21 2000 -- 1.37 -- 56 -- -- 318-22 2000 0.83 1.45.237 44 -- 1.29 29.5 4.37 318-22 700 0.78 1.48 -- 39 -- -- 318-23 2000 0.91 1.49 -- 54- -- 318-24 2000 0.97 1.29 -- 61 -- 1.49 -- 318-24C 2000 0.96 -- - - -- 25.0 4.47 318-26 2000 0.98 1.59 -- 70 -- 318-27 2000 0.87 1.38 - - - 318-28 2000 0.84 1.45.177.- - 1.33 -- 318-29 2000 0.63 1.45.194 26 -- -- 0.23 0.73 318-30 2000 1.08 1.49 -- 60 -- 1.52 21.9 5.82 318-31 2000 0.55 1.31.216 21 2.41 0.135 1.6 0.19 318-32 2000 0.84 1.57 -- 53 -- -- 19.7 -- 318-33 2000 0.80 --.101 57 0.73 1.37 32.2 4.75 318-34 2000 1.09 1.45 -- -- -- -- 28.7 4.85 318-35 2000 0.88 1.43 1.18 -- - 1.48 26.4* 4.57 318-36 2000 1.03 1.41 1.07 67 -- 1.35 18.6* 3.34 318-37 2000 0.92 1.48 1.12 -- -- 2.17 25.7* 3.90 318-38 2000 -- 1.52 --- -- --- 318-39 2000 1.24 1.57.85 -- -- 2.99 34.9* 7.95 318-41 2000 1.05 1.44 -- --- -- - 318-43 2000 1.08 -- -- 106- -- 318-44 2000 1.09 - -- 103 -- - 318-45 2000 1.27 --.39 -- - 3.1 -- 318-46 2000 1.02 --.41 56 -- 2.34 42.3* 7.35 318-48 2000 1.04 1.43 - -- - - 3.5 8.27 318-50 2000 —- - -- - -- -- 5.73 318-51 2000 0.88 1.43 -- -- - 0.83 17.3 1.44 *Head Speed.05 in/min., all others.02 in/min.

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. He Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xl0) (DPH) (x103) (xl1-6) (x10-3) (x10-3) 318-52 2000 1.01 1.41 1.30 -- - 1.66 17.7 2.54 318-53 2000 0.87 1.42 - - -- - 4.73 1.60 318-56 2000 0.85 1.34 --- -- --- 318-58 2000 0.98 -- 2.37 - -- 0.10 -- 6.02 318-59 2000 1.18 1.38 -- - -- 2.15 31.7 4.20 318-60 2000 0.95 1.71 1.50 54 -- 1.78 36.2* 7.63 318-61 2000 1.01 1.75.403 -- - 1.47 22.6* 3.96 318-62 2000 0.96 1.39 -- 69 -- 41.4 6.98 321-1B 2000 -- -- -- -- 4.36.87 321-3 2000 0.95 1.57.340 78 - -- 40.0* 7.18 321-5 2000 0.99 1.52 - - - 321-6 2000 1.09 1.60.31 81 -- 2.33 41.7* 8.27 321-7 2000 0.91 1.54 -- -- - - 321-8 2000 0.90 1.46.546 105 - 1.48 38.9* 7.00 321-9 2000 1.17 1.36 -- 120 - -- 54.2 9.75 321-10 2000 1.26 1.34 1.00 99 - 2.99 54.9* 10.85 321-11 2000 0.95 1.43 1.14 95 -- 1.54 40.5 5.16 321-11C 2000 -- -- -- 132 - - 37.0 6.08 321-12 2000 0.97 1.32 1.21 - - 1.22 14.9 2.52 321-13 2000 0.95 1.48 1.15 131 - 1.67 36.2 6.04 321-15 2000 0.96 1.56 - - - - 34.5 5.98 321-16A 2000 0.85 1.84 - - 0.21 1.55 24.3 4.52 321-16B 2000 0.93 1.75 - - 321-17B 2000 0.94 1.41 - - 0.22 1.81 36.7 5.26 321-18A 2000 0.95 1.67 321-18B 2000 0.64 - - - 0.2 1.73 39.6 5.67 321-19A 2000 0.87 1.68 - 115 0.15 1.83 31.5 6.04 321-19B 2000 0.83 1.80 - 87 0.11 1.49 31.4 5.76 321-20A 2000 0.99 1.72 -- - 321-20B 2000 0.70 1.50 - - - - 34.8 6.21 321-21A 2000 0.94 1.74.2 -- - 1.65 45.5 6.35 *Head Speed.05 in/min., all others.02 in/min.

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. PHe Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xl0) (DPH) (x103) (x10-6) (x10-3) (x10-3) 321-21B 2000 1.00 2.18.2 -- - 1.93 46.4 6.16 321-22A 2000 0.94 1.79.28 - - 1.44 31.9 6.14 321-22B 2000 0.98 -- -- - - -- 34.8 4.58 321-22C 2000 0.98 --.17 - - 1.43 36.1 4.35 321-22D4 2000 0.96 --.19 -- -- 1.42 33.7 5.15 321-23 2000 1.04 1.74.12 -- - 2.05 58.6 7.28 321-23A 2000 0.96 --.27 -- - 1.64 40.9 6.36 321-23B 2000 0.97 1.77.18 -- - 1.69 42.7 5.98 321-24 2000 0.92 --.19 -- -- 1.95 47.8 6.39 321-24A 2000 0.92 --.14 - -- 1.05 49.1 7.04 321-24B 2000 1.07 2.08.15 -- - 2.22 45.1 6.76 321-25A 2000 1.05 1.45X*.13 - -- 0.68 27.9 5.14 321-26 2000 0.50 1.43 - -- -- -- 26.4 0.77 321-26A 2000 0.45 1.54 -- -- 321-27 2000 0.86 1.52.11 -- - 0.62 9.7 1.34 321-29 2000 0.96 1.64.18 -- - 1.59 40.0 5.94 321-31 2300 0.81 1.41 -- -- -- 321-31A 2300 0.97 1.40 321-31B 2300 0.91 1.56 321-31C 2300 0.88 1.41 - -- 321-31D 2300 -- 1.98 - - -- -- 33.3 4.08 321-31F 2300 0.75 --.23 -- - 0.70 13.6 2.23 321-31G 2300 1.03 1.66.18 - - -- 22.2 3.53 321-31I 2300 1.02 1.48 -- -- -- 321-31J 2000 0.99 --.16 - - 1.15 22.6 3.99 321-31P 2000 0.93 --.24 - - 1.16 25.0 3.60 321-31Q 2000 1.01 1.29.17 -- -- 1.64 40.5 6.23 321-31R 2000 0.93 --.18 -- - 0.85 12.2 1.85 321-31S 2000 1.01 1.39.17 -- - 1.53 36.9 5.58 321-32A 2000 0.94 1.36.18 -- - 0.91 35.5 3.78 321-32B 2000 0.96 1.30.20 -- - 0.92 36.9 5.76 *Xylene, all others Helium.

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. PHe Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xlO) (DPH) (x103) x10-6) (x10-3) (x10-3) 321-32C 2000 0.95 1.25.21 - - 0.93 41.4 6.11 321-32D 2000 0.94 --.25 - 1.49 -- 321-32D1 2000 0.94 --.29 - - 0.2 -- 321-32E 2000 0.98 1.33.24 - - 1.56 41.9 5.89 321-32F 2000 0.96 -- - - - 0.91 33.3 4.28 321-32G 2000 0.99 --.22 -- - 1.56 31.8 4.53 321-33A 2000 0.97 1.41.16 - - - 39.8 5.96 321-33B 2000 0.89 1.30.33 - -- 1.49 53.6 6.69 321-34 2300 0.95 1.6 -- -- -- 321-34A 2300 0.92 1.59.27 - - 1.49 31.3 7.55 321-34B 2300 0.96 --.18 - - 2.94 33.3 2.92 321-34D 2300 0.99- -- - - 1.46 321-34E1 2300 0.97 1.21.38 -- - 0.92 40.9 5.43 321-36A 2300 1.11 1.80 - -- -- - 2.46 321-36B 2300 1.07 1.66.29 -- - 1.15 50.4 7.23 321-36C 2300 1.11 1.43 - -- 321-37 2300 1.07 1.44 -- 321-37B 2300 0.66 1.50.24 - - 0.42 5.53 1.09 321-37D1 2300 -- -- -- -- - -- 2.51 0.45 321-37E 2300 0.78 --.44 - - 0.94 1.39 0.36 321-37F 2300 0.68 1.56X - - - 0.08 1.05 0.22 321-37Q 2300 0.74 --.31 - - 0.2 1.67 0.40 321-39 2300 0.85 1.60.23 - - 0.72 6.80 1.31 321-40 2300 0.60 1.42.30 - - --- 321-41B 2300 0.77 1.51 -- -- -- 321-42A 2000 0.77 1.44X.29 - - 0.35 2.05 0.57 321-42B 2000 0.65 1.48.28 - - 0.20 1.14 0.42 321-43A 2200 0.76 1.55.36 -- - 0, 60 1.31 0.37 321-43B 2200 0.64 1.44.46 - -- 0.10 0.73 0.~2 321-44A 2200 0.96 1.81 -- -- -- 321-44B 2200 0.98 1.56 321-45A 2200 1.17 1.78 321-45B 2200 1.04 1.84 -

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. Papp. He Resistivity ness Frict. psi psi psi Sample #Temp.C (g/cc) (g/cc) Q-cm(xl0) (DPH) (x103) (x0l-6) (x0l-3) (x0-3) 321-46A 2200 0.83 1.40 -- -- -- 321-46B 2200 0.82 1.43.26 -- - 0.16 2.04 0.49 321-46C 2200 0.87 1.60 -- 321-47A 1600 1.13 2.07 321-47B 1600 1.18 1.67 321-47C 1600 0.91 1.84 321-48A 1600 0.79 1.40 -- -- -- 321-48B 1600 0.83 1.43.24 -- - 0.34 2.65 0.60 321-48C 2000 0.78 1.58 -- 321-49A 1600 0.91 1.51 321-49B 1600 0.80 1.44 321-49C 1600 0.91 1.51 321-50 1600 1.00 1.69 -- -- -- 321-50B 1600 1.02 1.43.15 -- - 1.5 28.2 4.52 321-50C 1600 1.03 1.45 -- -- -- 321-51 2350 0.99 1.50 -- -- - 0.73 9.1 1.36 321-51A 2350 1.01 1.53.21 -- -- 321-52 2000 -- 1.3 -- 321-53 2000 1.12 2.07 -- -- 322-1A 1600 0.77 1.59X.24 -- - - 4.00 0.78 322-1B 1600 0.77 1.98.39 -- 322-2A 1600 0.87 2.02 -- -- 322-3A 1600 0.78 1.59X.18 -- - 0.73 322-3B 1600 0.78 2.0 -- -- 322-5 2000 0.86 1.55 322-6 2000 0.86 1.41 322-10C 2100 0.84 1.8 -- -- 322-11A 1670 0.78 1.49X -- - - 0.25 322-11B 1670 0.78 1.9.26 - - 0.24 322-12A 1600 0.71 1.43X.28 - - 0.24 322-12B 1600 0.79 1.50X.23 - - 0.35 322-13A 1670 0.79 1.45X.17 - - 0.59 322-14A 1670 0.76 1.74 -- --

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. PHe Resistivity ness Frict. psi psi psi Sample #Temp.~ (g/cc) (g/cc) Q-cm(xlO) (DPH)(x1O3) (X106) (x1O3) (x103) 322-15B 1670 0.86 1.48X.19 - -0.57 322-16A 1670 0.81 1.89 -- -- 322-16B 1670 0.84 1.81X.22 - -0.35 322-17B 1670 0.76 1.71X.37 - -0.2 322-18A 1670 1.01 --.09 - -2.17 322-19A 1670 0.85 1.9 -- 322-19B 1670 0.89 --.28 - -0.33 322-20 1400 0.89 -.17 - -0.77 322-21 1400 0.81 —.22 - -0.53 -- 322-22A 1400 0.88 -- --- 4.1 1.19 322-22B 1400 0.89 1.49X- - -- 5.2 1.19 322-23A 1400 0.84 -- 322-23B 1300 0.83 2.03X- -- - - 4.07 322-24A 1300 0.87 1.74X- -- - - 1.28 322-24B 1400 0.82 1.59X- -- - - 1.28 322-25A 1410 0.88 —.11 - -1.56 322-25A 1670 0.88 —.13 - -1.48 322-26 1400 1.00 —.11 - -2.04 322-27A 1400 0.86 1.42X.08 - -1.58 -- 322-28A 1400 0.93 1.44X.10- - -- 18.4 3.16 322-29A 1400 0.69 1.46X.19 - -0.68 -- 322-30 1410 0.92 1.64.18 - -0.79 322-31B 1410 0.75 1.58X.34 - -0.24 322-32 1350 0.79 1.60X.24 - -0.36 5.8 0.79 322-33 1350 0.79 1.78X.22 - -0.60 -- 322-34 1350 0.88 1.34X.13 - -1.07 -- 322-35 1350 0.86 1.43X.22 - -0.68 11.8 1.33 322-36 1543 0.93 1.45X.10 -— 1.29 23.0 3.74 322-37 1543 0.82 1.46X.20 - -0.47 -- 322-38 1543 0.72 -.17 - -0.93 322-39 1440 0.84 —.18 - -0.72 322-40 1440 0.87 1.86X.11 - -1.14 322-41 1440 0.79 1.59X.17 - -0.84

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. Papp. PHe Resistivity ness Frict. psi psi psi Sample # Temp.~C (g/cc) (g/cc) Q-cm(xl0) (DPH) (x103) (x10-6) (x10-3) (x1-3) 322-42A3 1440 0.78 --.14 - -- 0.88 322-42A4 1440 0.73 --.23 -- - 0.68 322-42B1 1440 0.73 --.20 -- -- 0.69 322-42B2 1440 0.78 --.18 - -- 0.87 -- 322-42B3 1440 0.80 --.27 - -- 0.89 19.4 3.11 322-42B4 1440 0.73 --.17 - -- 0.70 -- 322-42B5 1440 0.74 --.19 -- - 0.76 322-42B6 1440 0.83 --.19 - -- 0.97 322-45 1440 0.91 1.72X.20 - -- 0.68 322-48 1605 0.73 --.29 - - 0.43 322-49A 1605 0.79 1.51X.15 - - 0.79 322-50 1600 0.79 --.15 - -- 0.56 322-51 1460 0.78 1.56 - -- -- 322-56 1500 1.00 1.48 322-56A 1500 0.96 1.33 322-57 1500 1.06 1.63 322-57A 1500 1.03 1.85 - -- 322-61 1500 0.79 1.50 -- -- - 0.4 322-62 1500 1.01 1.62 -- -- - 1.21 322-63 1500 1.03 1.56 - - -- 1.69 322-63A 1500 1.12 1.49 - - - 2.47 322-64 1370 1.00 1.60 - -- - 1.92 322-64A 1370 1.10 1.55 - - - 1.92 322-64B 1370 0.97 1.61 - - - 1.89 322-65 1370 1.28 1.45 - -- 322-66 1370 1.09 1.37 - -- 322-67 1350 0.85 1.64 - - - 1.32 322-67A 1370 0.84 1.65 - -- 322-67B 1370 0.86 1.84 - -- - 1.33 322-68 1370 0.78 1.52 - -- - 0.53 322-68A 1370 0.79 1.25 - -- 322-68B 1370 0.77 1.48 - -- 322-69 1370 0.76 1.50 - - - 0.42

Sonic Compr. Ult. Hard- Int. Mod. Str. Str. app. He Resistivity ness Frict. psi psi psi Sample # Temp.0C (g/cc) (g/cc) Q-cm(xl0) (DPH) (x103) (x10-6) (x10-3) (x10-3) 322-69A 1370 0.76 1.56 -- - - 0.42 322-70 1370 0.69 1.56 -- - -- 0.38 323-1 1370 1.01 1.47- --- 323-2 1370 0.81 1.51 - - - 1.15- 323-2A 1370 0.73 1.50 - - -- 1.30 323-3 1370 0.98 1.36- -- - 323-3A 1370 1.13 1.61 - - -- 2.48 323-4 1370 0.78 1.49 - - - 0.55- 323-4A 1370 0.76 1.49 - - -- 0.55 - 323-8A 1000 0.95 1.52 o00 Il

TABLE 9 Physical Properties Correlated with Density E/P a/ /P a _/P E H_ CE He cHe sPapp. cs/Papp. UTS/Papp. spa-ep =sP ] es UTSPp I PHe] app. P pp. c app, app. Sample # in(x10-6) in(x10-3) in(x10-3) psi(xl0-6) psi(xl0-3) psi(x10-3) Q-cm(xl0) 310-35 -- 252.4 49.2 311-34 -- 333.3 325.9 311-35 19.2 37.2 66.9 312-13 -- 1298.0 125.9 - ----- 312-14 -- 1000.0 -- - 51.8 -- 312-16 -- 624.0 102.1 -- 28.5 4.67 312-27 - -- 188.0 -- -- 312-29 -- 1030.6 -- -- 56.4 312-32 -- 901.2 158.3 -- 47.7 8.38 312-34 -- 824.2 33.5 -- 40.9 1.09 312-49 -- -- 150.5 -- -- 7.04 1 315-2 50.3 58.5 14.3 2.76 3.2 0.78.016 315-14 -- 1235.5 136.0 -- 71.2 1.04 315-17 -- 1030.0 88.3 -- -- -- 315-20A 48.8 -- -- 2.82 315-20B 49.3 -- -- 2.85 -- -.013 315-20C 48.1 -- -- 2.76 -- -.009 315-21B -- -- 191.0 -- -- 315-21C 45.8 1428.6 217.6 2.51 78.2 11.9.009 315-21D -- 743.0 209.5 -- -- -- 315-25A -- 767.0 145.5 - 315-25B -- -- 152.6 -- --- 315-25C 48.8 1120.5 232.9 2.41 56.9 11.8.020 315-26B -- 962.8 209.3 -- 315-26C 41.7 888.9 147.2 2.18 46.4 7.7.003 315-26D 46.2 1224.9 -- 2.34 63.9 --.009 315-28 -- 1079.3 127.0 -- 56.7 6.68 315-31B 50.0 1218.8 178.8 2.63 63.4 9.4.007 315-31C 49.3 -- -- 2.63 -- --.015 315-31D 48.8 1105.0 201.5 2.56 58.1 10.6.014 315-32 -- 1262.6 178.2 -- 65.0 9.2

/p e IPHe IP HP E /P /P /P E fT p pa1 s app. cs app. UTS app. s Papp csP UTS pp app.app aHe Sample # in(x106) in(x10-3) in(xl103) psi(xl0-6) psi (x0-3) psi(xl0-3) Q-cm(xlO) 315-33 44.9 -- -- 2.42 -- --.010 315-34C 40.3 972.2 136.6 2.29 55.3 7.7.011 315-34D 51.5 690.2 114.9 2.91 39.0 6.5.006 315-37 31.9 744.2 131.6 1.85 43.1 7.6.009 315-38A 35.9 925.9 114.6 1.95 50.3 6.2.011 315-39A 51.5 1038.8 161.7 3.03 61.3 9.5.011 315-39B 51.0 824.7 127.6 3.01 48.7 7.5.002 315-41 -- 612.8 -- -- 36.8 --.009 315-41A 48.7 671.0 72.2 2.93 40.3 4.3.002 315-41B 45.9 563.0 69.9 2.69 33.8 4.3.007 315-42 52.7 -- -- 3.47 -- --.012 315-43 -- 1335.5 -- -- 91.3 - 315-44 52.1 -- -- 3.34 - --.009 315-45B 211.9 -- -- 10.6 -- --.002 315-46A -- 2.78 2.48 -- 4.4 3.9 317-1 -- 1297.1 172.2 -- 77.9 10.4 317-2 35.6 922.0 116.2 2.23 55.1 7.3.004 317-5 -- 1175.0 266.0 -- 56.1 13.7 317-8 56.2 1247.0 70.5 3.32 73.8 4.17 317-9 -- 964.8 172.3 -- 61.1 10.9 317-10 50.9 1536.6 210.9 2.61 78.5 10.8.001 317-12 -- -- 181.6 -- -- 10.5 317-14 -- 874.8 149.7 -- 46.9 8.03 317-15 -- 1025.6 124.8 -- 53.9 6.6 317-18 33.0 126.0 104.0 1.79 10.6 6.9.004 317-19 -- 693.2 215.1 -- 41.9 13.0 317-23 -- 254.0 63.4 -- -- 317-24 52.9 1794.6 159.7 2.99 101.4 9.0.009 317-25 -- 1076.4 89.9 -- 65.5 5.5 317-26 53.7 167.4 32.8 2.86 8.9 1.7.010 317-29 32.3 615.0 92.8 1.92 36.6 5.53.009 317-32 51.3 1380.0 113.0 3.17 85.4 7.0.012 317-33 -- 1092.0 152.0 -- 57.5 8.0

/p~ a/p a /pEIe IHe a e I a I E /P Cr /P cr /P E PHe ap p H p s app. csapp. UTSapp. SPapp csp J UTSp J HeP Sample # in(xl0-6) in(xl0-3) in(xl0-3) psi(x10-6) psi(xl0-3) psi(x10-3) Q-cm(xl0) 317-34 88.4 1025.6 197.0 4.97 57.6 11.1.013 317-37 49.8 1049.0 212.0 2.40 60.4 10.3.015 317-38 31.3 1158.0 126.0 1.47 54.76 6.11.018 317-39 43.3 963.0 129.0 1.98 44.0 5.9.002 317-40 40.7 736.0 111.0 2.15 38.9 5.9.011 317-41 -- 298.0 70.0 - -- --- 317-41A -- 228.0 58.8 317-41B -- 668.0 96.5 -- 35.7 5.15 317-42 49.1 1266.0 169.0 2.63 66.3 8.8.008 317-43 -- 462.0 76.0 -- 23.4 3.84 317-44 44.6 903.0 70.4 2.43 4.91 3.83.0004 317-45 -- 1017.0 164.0 -- 51.4 8.3 317-46 43.5 1183.0 215.0 2.32 63.2 9.7.006 1 317-47 -- 785.0 160.0 -- 39.3 8.05 ao 317-48 29.9 -- 1.57- - 317-49 30.8 385.4 104.2 1.67 20.9 5.7.018 318-1 24.8 -- 89.8 1.35 -- 4.9.009 318-2C 25.0 1076.8 148.9 -- - - 318-7 23.2 29.2 28.0 -- -- 318-8 -- 526.6 162.6 -- 28.2 8.7 318-8A -- 936.4 ---- -- - 318-9 -- 792.8 150.2 -- 42.8 8.1 318-11 45.3 -- 155.0 2.58 -- 8.8 318-14 14.6 170.9 29.9.76 9.0 1.6.015 318-16 42.3 831.0 118.0 2.26 44.4 2.3.017 318-17 44.2 1246.2 163.0 2.66 65.5 8.51.019 318-22 43.2 987.0 146.0 2.25 51.5 7.63.014 318-24 42.5 -- -- 1.97 - --- 318-24C -- 715.0 129.0 -- -- 318-28 43.9 -- -- 2.30 -- --.010 318-29 -- 10.1 32.2 --.5 1.7.008 318-30 39.2 563.3 149.62 2.10 30.2 8.03 318-31 6.8 80.3 9.6.32 3.8.5.009

{ e i (He T He ] [Pa l app. csaps/Papp. app. app.c. Sample # in(xl0-6) in(xl0-3) in(xlO-3) psi(xl0-6) psi(x10-3) psi(x10-3) Q-cm(xlO) 318-32 -- 650.0 -- - 36.5- 318-33 46.9 1118.1 164.9. -- 318-34 -- 729.0 123.0 -- 38.2 1.13 318-35 46.9 831.0 144.0 2.41 42.9 7.4.070 318-36 42.6 573.0 103.0 2.12 29.13 5.2.078 318-37 65.7 773.0 117.0 3.50 41.3 6.3.070 318-39 64.9 778.0 178.0 3.7 44.2 10.1.007 318-45 67.6 - -- -- --- 318-46 62.7 1149.0 200.0.318-48 -- 93.2 220.0 -- 4.9 --- 318-51 26.0 546.0 45.3 4.23 28.2 2.3 -- 318-52 46.2 486.8 69.9 2.35 24.7 3.55.009 318-53 -- 151.0 51.1 -- 7.9 2.7 -- 318-58 2.8 -- 165.0- - - 0 318-59 50.6 744.0 98.6 2.51 39.8 -- 318-60 52.0 1055.0 222.0 2.2 65.2 13.7.079 318-61 40.4 620.0 109.0 2.55 39.2 6.9.023 318-62 -- 1195.0 201.0 -- 60.2 10.1 -- 321-3 -- 1166.0 209.0 -- 66.1 11.9.021 312-6 59.5 1061.0 210.0 3.43 61.3 12.1.021 321-8 45.6 1197.0 215.0 2.39 63.1 11.4.034 321-9 -- 1283.0 231.0 -- 63.0 11.3 -- 321-10 66.0 1207.0 238.0 3.18 58.4 11.5.009 321-11 44.9 1184.0 151.0 2.36 60.9 7.77.076 321-12 35.0 427.0 72.0 1.67 20.3 3.4.089 321-13 48.7 1032.0 176.0 2.59 56.4 9.4.074 321-15 -- 994.00 173.0 -- 56.1 9.7 -- 321-16A 50.7 792.0 148.0 3.36 52.6 9.8 -- 321-17B 53.5 1089.0 155.0 2.71 55.1 7.9 -- 321-18B 80.1 1726.0 246.0 -- 321-19A 58.4 1006.0 193.0 3.53 60.8 11.7 -- 321-19B 49.9 1055.0 192.0 3.23 68.1 12.5 321-20B -- 1381.0 246.4 -- 74.6 13.3

E[/P P E HeI [He r He _ s/Papp. cs/app. OUTS/Papp. Papp. s P app JUTS pppHe Sample # in(x10-6) in(x10-3) in(x10-3) psi(x10-6) psi(x10-3) psi(x10-3) -cm(x10) 321-21A 48.8 1344.6 187.6 6.03 86.6 12.1.011 321-21B 53.6 1288.9 171.1 4.21 101.2 13.4.009 321-22A 42.6 943.0 181.0 2.74 60.7 11.7.014 321-22B -- 986.4 129.8 -- 54.7 7.2 -- 321-22C 40.5 1023.2 123.3 2.2 55.3 6.7.007 321-22D4 41.1 975.1 149.0 2.2 51.6 7.9.010 321-23 54.8 1565.0 194.0 3.4 98.0 12.2.008 321-23A 47.5 1183.4 184.0 2.6 65.2 10.1.017 321-23B 48.4 1222.8 171.0 3.1 77.9 10.9.010 321-24 58.9 1443.0 193.0 3.4 83.1 11.1.011 321-24A 31.7 1482.5 212.6 -- -- -- -- 321-24B 57.6 1170.8 175.5 4.3 87.7 13.1 -- 321-25A 18.0 738.0 136.0.94 38.5 7.10.009 1 321-26 -- 1466.7 42.8 -- 75.5 2.2 -- oo 321-27 20.0 313.3 43.3 1.2 17.1 2.4.006 oo 321-29 46.0 1157.0 172.0 2.7 68.3 10.1.011 321-31F 26.0 503.8 82.6 1.6 30.5 5.0.010 321-31G -- 599.0 95.2 -- 36.0 5.7.011 321-31J 32.3 634.0 112.0 1.72 33.8 5.96.011 321-31P 34.6 747.0 108.0 1.56 33.6 4.8.018 321-31Q 45.1 1114.0 171.0 2.09 51.7 7.96.013 321-31R 25.4 364.4 55.3 -- -- -- -- 321-31S 42.1 1104.9 153.5 2.11 50.8 7.68.012 321-32A 26.9 1049.0 111.7 1.36 51.4 5.47.012 321-32B 26.6 1067.7 166.7 1.25 50.0 7.80.015 321-32C 27.2 1210.5 178.7 1.22 54.5 8.04.016 321-32D 44.0 -- - -- -- -- -- 321-32D1 5.9 -- -- -- -- -- 321-32E 44.2 1187.6 166.1 2.12 56.9 7.99.018 321-32F 26.3 963.5 123.8 1.46 53.4 6.9 -- 321-32G 43.8 892.3 127.1 -- -- -- 321-33A -- 1139.7 170.7 -- 57.9 8.66.011 321-33B 46.5 1673.0 208.8 2.18 78.3 9.77.023

a s a^ep P 1 s/Papp. cs/Papp. aUTSa/PEapp. s [Hp e Cs:1H 1 UTS p I[.P ap app. app. TSapp. He Sample # in(xl0-6) in(x10-3) in(xl0-3) psi(x10-6) i lpsi(x103 psi(x0-) Q-cm(x10) 321-34A 45.0 945.0 228.0 2.6 54.1 13.0.016 321-34B 85.1 963.5 84.5 -- -- 321-34D 41.0 -- - 321-34E1 26.0 1171.2 155.5 1.15 51.0 6.77.030 321-36A- -- 61.6 - -3.99 321-36B 29.9 1308.0 187.7 1.78 78.2 11.2.019 321-37B 17.7 232.7 45.9.95 12.6 2.5.011 321-37E 33.5 49.5 12.8 2.12 3.1.81.020 321-37F 3.3 42.9 8.9.18 2.41.50 321-37Q 7.5 62.7 15.0.44 3.6.9.012 321-39 23.5 222.2 42.8 1.4 12.8 2.5.013 321-40 -- -- -- - --.013 321-42A 12.6 73.9 20.6.65 3.83 1.07.012 321-42B 8.5 48.7 17.9 4.6 2.6.96.012 oo 321-43A 21.9 47.9 13.5 1.2 2.7.75.018 321-43B 4.3 31.7 9.5.23 1.6.5.020 321-46B 5.4 69.1 16.6.28 3.6.85.015 321-48B 11.4 88.7 20.0.6 4.6 1.0.014 321-50B 40.8 769.9 123.0 2.1 39.5 6.3.011 321-51 20.5 255.0 38.2 1.1 13.8 2.1 -- 321-51A -- -- -- -- --.014 322-1A 9.74 144.3 2.81.56 8.3 1.6.012 322-1B 9.38 -- —.67 -- --.015 322-3A 26.0 -- 1.49 --.009 322-1A 8.9 - --.48 - 322-11B 8.5 -.58- -.011 322-12A 9.4 --.48 --.014 322-12B 12.3 - --.66 --.012 322-13A 20.7 -- 1.1 --.009 322-15B 18.4 - —.98 --.011 322-16B 11.6 --.75 --.010 322-17B 7.3 --.45 --.016 322-18A 59.7 --

PHee Ple [ PClHe s/Papp. cs/Papp. UTS/Papp. S (Papp s sp UTS p e] [.P app. app. Sample # in(x0-6) in(x10-3) in(x10-3) psi(x10-6) psi(x10-3) psi(x10-3) -cm(xlO) 322-19B 10.3 - --- - 322-20 24.0- -- - 322-21 18.2 - -- -- 322-22A -- 129.4 37.6 - 322-22B -- 162.3 37.1 -- 8.71 1.99 322-23B -- 136.2 - -- 10.20 322-24A - -- 40.9 -- - 2.56 322-24B -- -60.3 - - 2.48 322-25A 49.2 -- -- 322-25A 46.7 322-26 56.7 - -- - 322-27A 51.0 -- -- 2.61 -- -.005 322-28A -- 549.6 94.4 -- 28.5 4.89.006 322-29A 27.4 -- - 1.44 - -.009 322-30 23.9 - -- 1.41 -- -.010 322-31B 8.9 - --.51 -- -.016 322-32 12.7 203.9 27.8.73 11.75 1.6.012 322-33 21.1 - - 1.35 -- -.010 322-34 33.8 -- -- 1.63 - --.009 322-35 21.9 381.0 43.0 1.13 19.6 2.2.013 322-36 38.5 686.9 111.7 2.01 35.9 5.83.006 322-37 15.9 -- -.84 - -.011 322-38 35.9 - -- -- 322-39 23.8 - -- - 322-40 36.4 -- - 2.44 -- -.005 322-41 29.5 - - 1.69 - -.008 322-42A3 31.3 - -- - 322-42A4 25.9 322-42B1 26.3 322-42B2 31.0 -- -- - 322-42B3 31.0 673.6 108.0 322-42B4 26.6 -- -- -- 322-42Bs 28.5 -- -

E/P cr a!He.j He crF He r s app. cs /Papppp. UTS a pp. s (p. UTS ( app P app. app. app. c Sample # in(x10-6) in(x10-3) in(xl0-3) si 6psi(x10-6 ) psi(x10-3) psi 3) -cm(xlO) 322-42B6 32.5 - -- - 322-45 20.8 -- -- 1.28 -- -.011 322-48 16.4 - -- - 322-49A 27.8 - -- 1.51 -- -.008 322-50 19.7 - -- - 322-61 14.1 - --.8 322-62 33.3- -- 1.9- - 322-63 45.6 - -. 2.6- - 322-63A 61.3 -- - 3.29 322-64 53.3 -- 3.65 - 322-64A 48.5 -- 2.7 322-64B 54.1 -- 3.14 322-67 43.1 - — 2.5- 322-67B 42.9 -- -- 2.8 w 322-68 18.9 ---- 1.0 - - 322-69 15.4 ---.8- -- 322-69A 15.4 - —.8 322-70 15.3 --—.9 323-2 39.4 - -. 2.1- - 323-2A 49.5 -- -- 2.7 323-3A 61.0 --- 3.5 - 323-4 19.6 ---- 1.1 - 323-4A 20.1 -- -- 1.1

TABLE 10 Comparison of Ultimate Strength Determined by Direct Tension vs. Disc Rupture Sample # Direct Tension Disc Rupture 317-38 3780 psi 5100 psi 318-59 4600 psi 4153 psi 321-16B 5306 psi 4705 psi 321-36A 4081 psi* 2462 psi 321-50B 3780 psi 5228 psi 322-23B 3163 psi 4050 psi 322-24A 1367 psi 1279 psi 322-24B 1122 psi 1279 psi *Broke in Grip TABLE 11 Comparison of Sonic Modulus and Mechanical Modulus HTT Sample # Temp.~C Mechanical Modulus Sonic Modulus 317-8 2000 1.27 x 106 1.82 x 106 317-26 2000 0.38 x 106 0.31 x 106 317-42 2000 1.4 x 106 1.5 x 106 317-46 2000 1.59 x 106 1.27 x 106 318-17 2000 1.16 x 106 1.18 x 106 318-52 2000 2.0 x 106 1.69 x 106 321-12 2000 1.01 x 106 1.22 x 106 -92

TABLE 12 Sonic Modulus vs. Pyrolysis Temperature psi(xl0-6) Sample # 700~C 800~C 9000C 1000~C 1577~C 1800~C 2000~C 318-59 #lL 1.02 -- -- 2.16 1.95 1.77 1.46 318-59 #2L 1.06 -- -- 2.07 2.10 1.82 1.76 318-60L.93 - -- 1.82 1.77 1.70 321-11L.75 -- 2.37 1.68 1.72 1.58 321-llCL.73 -- -- 1.75 1.75 1.72 1.66 321-12L.66 -- 1.49 2.03 1.23 1.18 321-13 #lL.80 -- -- 1.84 1.77 1.73 1.75 321-13 #2L.82 -- -- 1.84 -- 1.79 1.72 321-13 #3L.88 - -- 1.91 -- 1.75 1.72 321-15 #1.81 -- 1.69 1.92 1.91 1.84 1.69 321-15 #2 -- 1.53 -- 1.96 2.01 1.86 1.71 321-15L -- 1.69 -- 2.06 1.875 1.86 1.79 321-16A -- 1.60 -- 1.88 1.87 1.70 1.55 321-16AL -- 1.57 -- 1.97 1.87 1.67 1.58 321-16B -- 1.68 -- 1.87 1.68 1.55 1.48 321-17B.80 -- 1.80 2.12 1.96 1.91 1.81 321-18A -- 1.63 -- 2.2 2.14 2.09 1.98 321-18B #1 -- 1.73 -- 1.48 1.86 1.81 1.73 321-18B #2 -- 1.52 -- 1.97 2.09 1.74 1.73 321-18BL -- 1.56 -- 1.60 1.90 1.83 1.75 321-19A -- 1.53 -- 2.03 1.96 1.89 1.83 321-19B #1.75 -- 3.27 1.58 1.78 1.49 1.49 321-19B #2 -- 1.32 -- 1.69 1.61 1.61 1.55 321-19BL -- 1.40 -- 2.15 1.63 1.64 1.55 -93

TABLE 13 Resistivity vs. Pyrolysis Temperature Q-cm(xlO) Sample # 800~C 900~C 1000~C 1577~C 1800~C 2000~C 318-59 #1L -- --.499.102.083.110 318-59 #2L -- --.522.099.081.060 318-60L --.523.0108.016.170 321-11L -- --.643.116.120.120 321-11CL -- --.471.098.090.170 321-12L -- --.542.148.120.06 321-13 #L -- --.506.120.170.100 321-13 #2L -- --.521.106.160.110 321-13 #3L ----.490.111.110.110 321-15 #1 --.143.014.0302.015.015 321-15 #2.448 --.029.0319.015.015 321-15L.324 --.110.115.170.110 321-16A.279 --.014.029.015.015 321-16AL.366 --.170.089.120.100 321-16B.445 --.030.0328.017.017 321-17B --.083.080.0357.018.018 321-18A.238 --.047.0333.017.017 321-18B #1.611 --.059.0334.016.016 321-18B #2.302 --.03.0325.016.016 321-18BL.374 --.160.114.110.110 321-19A.317 --.031.0332.017.017 321-19B #1 --.171.017.0368.018.018 321-19B #2.302 --.03.0325.016.016 321-19BL.355 --.150.081.110.110 -94

UNIVERSITY OF MICHIGAN 3 90111111 1 126 306111111 3 9015 03126 3067