SHRP-ID/UFR-92-610

The Use of Conversion Residue as a Component in Cement

Richard E. Root, P.E. Chicago Testing Laboratory, Inc. 3360 Commercial Avenue Northbrook, IL

Richard B. Moore Shell Development Company P.O. Box 1380 Houston, TX

Strategic Highway Research Program National Research Council Washington, DC 1992 SHRP-ID/UFR-92-610 Contract ID-020

Program Manager: Edward Harrigan Project Manager: Rita Leahy Production Editor: Amy Gray Light Program Area Secretary: Juliet Narsiah

June 1992 Reprint December 1993 key words: asphaltic concrete conversion residue thermal cracked residues thermal

Strategic Highway Research Program 2101 Constitution Avenue, N.W. Washington, D.C. 20418

(202) 334-3774

The publication of this report does not necessarily indicate approval or endorsement of the findings, opinions, conclusions, or recommendations either inferred or specifically expressed herein by the National Academy of Sciences, the United States Government, or the American Association of State Highway and Transportation Officials or its member states.

© 1993 National Academy of Sciences

50/NAP/1293 Acknowledgments

The research described herein was supported by the Strategic Highway Research Program (SHRP). SHRP is a unit of the National Research Council that was authorized by section 128 of the Surface Transportation and Uniform Relocation Assistance Act of 1987.

olo lU Contents

Abstract ...... 1

Executive Summary ...... 2

Related Research ...... 4

Binder Preparation ...... 4

Binder Evaluation ...... 5

Methodology of Binder Evaluation ...... 5

Arabian Heavy ...... 7

California Heavy ...... 7

Binder Evaluation in Bituminous Mixture ...... 8

Arabian Heavy ...... 9 Georgia Aggregate ...... 9 Maryland Limestone ...... 10 Texas Chert ...... 10 Comments ...... 10

California Valley ...... 10

Conclusions and Recommendations ...... 11

Appendix A List of Figures ...... 12

Appendix B List of Tables ...... 24

References ...... 104

V Abstract

Thermal cracking of distilled residues was a popular refining practice in the 1920s that helped double the production of from a given quantity of crude oil from 1919 to 1935. Thermal cracked residues, a by-product of thermal cracking, were used as paving materials in the 1920s and '30s, although they ultimately proved unsatisfactory for this purpose.

A conversion residue generally used as a blending component in heavy fuel oils or as a refinery fuel, was discovered to successfully blend into paving grade asphalt to provide superior resistance to moisture-induced damage, and to provide similar hardening characteristics as conventional specification asphalt.

Although conversion residue is seldom used in the United States, the preliminary findings of this material compared to conventional asphalt form the basis of this SHRP IDEA study. Executive Summary

Thermal cracking of distilled residues became a popular refining practice in the 1920s. The primary benefit of thermal cracking was to increase the production of gasoline and other light products from a given quantity of crude, and decrease the volume of asphaltic residue. As a result of the introduction of thermal cracking, the production of gasoline from a given quantity of crude oil was practically doubled during the period of 1919 to 1935 (ref 1).

Thermal cracked residues (TCR), a by-product of thermal cracking, were used as paving materials in the 1920s and '30s. Most of the TCR, however, was volatile (not highly vacuum distilled), and proved to be unsatisfactory in terms of age hardening (partially due to high volatility losses during the hot mix process to make asphaltic concrete). This led to some premature failures (primarily thermal and fatigue cracking) of pavements.

The Oliensis spot test (ref 2), developed in 1933 as a means of identifying TCR, was later used as a specification standard to ensure that TCRs were not used in paving . (This test is still mandatory in eight states and optionally enforced in 21 states-- AASHTO M226, Table 2) (ref 3). The thin film oven test (TFOT), developed in 1941, gave a more accurate prediction of age hardening during plant mixing to produce hot mix asphaltic concrete (ref 4). A majority of states today no longer run the spot test, while all use the TFOT, or rolling thin film oven test.

Conversion Residue (CR) is a visbroken material (lightly thermal cracked, typically exposed to temperatures between 420C and 480C) that is subjected to a high vacuum to remove volatile materials (ref 5). CR is produced according to the scheme illustrated in Figure 1, page 13. If the material exiting the visbreaking reactor is not exposed to a high vacuum unit, the resulting residue would be volatile, a poor aging material, and would be classified as visbroken residue--not CR.

CR is generally used as a blending component in heavy fuel oils or as a refinery fuel, and it has a relatively low value when compared to other refinery streams. If CR were to be blended into paving grade asphalts, it would not increase the overall cost of the asphalt. Presently, CR is seldom (if ever), used in paving grade asphalts in the United States. However, previous preliminary findings (ref 6) show that when CR is used in small percentages, (< 20 percent) with the remainder being a conventional distilled asphalt, the resultant material in limited testing displayed superior resistance to moisture-induced damage (Modified Lottman Test) and similar hardening characteristics

2 (TFOT) when compared to conventional specification asphalts. These preliminary findings are the basis of this SHRP IDEA study.

For this study, two different CR materials, two sources of vacuum distilled asphalt, and three sources of aggregate were evaluated. The asphalts and their blends were tested using standard specification binder tests, and the asphalt-aggregate mixtures were tested using ASTM-D-4867 (ref 7) to assess moisture-induced damage. RELATED RESEARCH

The reduction of moisture-induced damage by using CR or TCR is not widely known or practiced in the United States. However, in the 1955 Proceedings of the Association of Asphalt Paving Technologists (AAPT) there is a paper entitled "Waterproofing Aggregates with Cracked Road Oils" (ref 8). The authors concluded "that certain cracked road oils are better waterproofing agents than any other commonly used asphalt products".

In the 1988 Proceedings of AAPT a paper entitled "Hydrocracking Residues--The Potential Source of Road Binders" by Zanzotto et al (ref 9) showed dramatic improvement in percent of retained Marshall stability after a 24-hour soak with as little as 3_ hydrocracked residue. Zanzotto also showed lower aging index values with 20_ or less hydrocracked residue in the blend when compared to the straight run asphalt. At percentages above 30_ the hydrocracked residue increased the aging index significantly.

In work done at Shell Development (ref 6) findings similar to Zanzotto's were reached when CR was used. A blend containing 17.6_ CR had a lower aging index than the original vacuum distilled AC-5 blending base. Also, a blend having 20% CR had a higher Tensile Strength Ratio (51.2I vs. 36.1_) when compared to the control (using the Modified Lottman Test procedure as run by the Texas State Department of Highways and Public Transportation).

BINDER PREPARATION

Two CR materials were chosen. One sample (W-834) is a Tia Juana Pesado (TJP) CR. TJP is Venezuelan crude. The other (W-840) is a Middle East CR. Asphalt sources chosen from the SHRP Materials Reference Library (SHRP MRL) were Arabian Heavy (AAS) and California Valley (AAG). West Texas Intermediate (solvent deasphalted) (AAM) was originally chosen, but proved to be incompatible with both CR materials. This was determined by viewing thin films of the blends under a microscope at 200X. Instead of being a homogenous honey color (compatible), these blends contained a network of visible black structures (flocculated asphaltenes). All subsequent blends used in this study were compatible using the 200X microscopic technique.

It was the aim of the study to have CR blended at O, 5, 10, 20 and 40% by weight of the total binder with the base asphalt; and the resultant blends have a consistency of AC-20. The AC-20 blends (18 in all) were then tested using common asphalt specification tests along with a minimum of other tests that have shown some correlation to field performance.

Because both CR materials were more viscous than AC-20, it was necessary to use a soft asphalt to give the resultant blends the proper consistency. The softest California Valley available from the SHRP MRL was an AR-2000 and for the Arabian Heavy an AC-IO. In a few of the higher Z CR blends, soft asphalts were not sufficient, and a heavy non-volatile distillate from a Mexican/West Texas Sour crude was used to attain AC-20 consistency. BINDER EVALUATION

Binder tests results are found in Tables IA through 4A. Calculated properties of the binders are found in Tables IB through 4B. It should be noted that all blends did meet AASHTO M-226 specifications for either AC-20 Table I or Table 2, except (in some cases) for the optionally specified Spot Test.

METHODOLOGY OF BINDER EVALUATION

The following calculated properties and test data are considered important in predicting binder performance:

Bitumen Temperature Susceptibility (BTS) Estimated Thermal Cracking Temperature (ETCT) Penetration at 4C (60 seconds, 200 _rams) Viscosity at 60C of Original penetration Aging Index Exudation 0roplet Tests (EDT)

It is more meaningful to evaluate these properties or data on TFOT residue (where applicable), because TFOT residue closely matches the short-term aging that occurs during construction of a hot mix asphalt pavement (ref I0). Unfortu- nately, at the time of this study there was no standard long-term aging test available (Pressure Air Vessel test under development in SHRP). Each of the above properties and test data in relation to performance are discussed below.

BTS is identical to the Penetration Index (PI) as developed by Pfeiffer and Van Doormaal (ref 11) when penetrations are used. Heukelom (ref 12 & 13) extended the PI concept to include viscosities. However, PI based on viscosities is a contradiction in terms, and authors de Bats and van Gooswilligen (ref 14) developed the term BTSwwhi_h will be used in this report. From a rheological standpoint it would be advantageous to have a relatively stiff binder at high service temperatures (high viscosity at 60C) and a relatively soft binder at low temperatures (high penetration at 4C). This type of material would have a high BTS value. BTS can be represented graphically using the Bitumen Test Data Chart (BTDC) developed by Heukelom (ref 12). An example of the BTDC is given in Figure 2. Three classes of asphalt are shown: Type W (waxy), Type S (straight line) and Type B (blown). The slope of the line in the performance region (typically 60C and below) is of most concern. Viscosities (and BTS) at temperatures above the performance region are important during the construction of the pavement, but once properly constructed, they have no correlation to performance.

ETCT is based on findings of low temperature thermal cracking from the ST. Anne's Test Road (ref 15). A relatively simple chart (see Figure 3) and penetrations at 5C and 25C are all that is needed to determine the ETCT. Penetrations ( 5 seconds and 100 3rams) were run at4C and 25C in this study. The penetration at 5C was interpolated (using BTDC) and used in calculation of the ETCT.

The Pacific Coast Conference on Asphalt Specifications has adopted the 60 second- 200 gram penetration test at 4C on Rolling Thin Film Oven Residue in their 1990 Performance Based Asphalt Specifications. It is felt that this test is better

5 from a precision standpoint than the 5 second -100 gram test at 4C. The apparent problemwith the 5 second test at low temperatures is the depth of penetration is small, and it is on the highly tapered portion of the needle. Goodrich (ref 16) evaluated the 60 second penetration test at 4C as a performance based test, and found that it correlated with low temperature creep testing on mixtures (limiting stiffness temperature) better than any other binder test in his study.

Viscosity at 60C is the basis of our country's present Viscosity Graded Asphalt Cement Specifications. It is intuitively obvious that the higher the viscosity of the asphalt cement--the stiffer the mixture, and the more resistance the mix is to permanent deformation (rutting). The Shell Pavement Design Manual (ref 17) has input parameters for asphalt cement stiffness, and this factor directly affects predicted mix stiffness and rutting.

Percentage of original penetration (25C) after the TFOT is a specification requirement for Penetration Graded Asphalt Cements (ref 18). AASHTO M-20 requires a minimum of 58X, 54_ and 50_ for 40-50, 60-?0, and 85-100 penetration grades. If the % is less than these minimums, then it is inferred that the material is prone to excessive aging and the resulting pavement will prematurely crack.

Aging index is the ratio of TFOT viscosity • 60c / viscosity e 60c. AASHTOM-226 limits this ratio to a maximum of 4.0. If the aging index is above 4.0, then (similar to I of original penetration) it is inferred that the material is prone to excessive hardening during aging and the resulting pavement will prematurely crack. However, pavements do notcrack at BOCmthey crack at lower temperatures; and the fallacy of the aging index was discussed by Moore (ref 19). In this • discussion it was pointed out •that some aged asphalts develop high 60C viscosities, but they have excellent low temperature properties (high 4C penetrations--soft and resistant to cracking}. It was concluded that judging how an asphalt will perform after age hardening cannot be adequately assessed by only comparing relative aging indexes based on viscosities at 60C.

The exudation droplet test (EDT) was proposed by van Gooswilligen, de Bats and Harrison (ref 20). It has been found that exudative hardening may contribute to premature fracture of pavements, which occurs more frequently with lean mixes. Exudative hardening is the loss of oily material that exudes from the binder into the mineral aggregate. Shell Method Series 2697 was the test procedure followed. Weighed quantities of asphalt are placed in drilled recesses of a marble plate of a specific Italian origin. The plates are heated to 60C for four days under a nitrogen blanket. During this period oily rings develop which are measured with a microscope under ultraviolet light. For AC-20 materials a ring width of less than 2.0mm is an indicator_9ood performance. All blends in this study were 1.2mm or less.

The following two sections will discuss how the two CRs affected the Arabian Heavy and California Valley asphalts.

6 ARABIAN HEAVY

Arabian Heavy is recognized as an asphalt with low temperature susceptibility, and because of this is generally considered a gocx_ performer. It easily exceeds AASHTON-226 Table 2 require_nts for temperature susceptibility (minimum 60 penetration at 25C and 1600 to 2400 poise at 600). The ArebianHesvy AC-20 has a 25C penetration of 81 and a 60C viscosity of 2041 poise (Table 1A) and a BTS of -0.73 (Table 1B). It can be seen that both CRs had little effect on the BTS (25C pen. & 60C visc.) for original properties (Table 1B & 2B). However, in all cases CR improved the BTS after the TFOT when compared to the control AC-20.

BTS (4C pen & 60C visc.) for the control AC-20 (Table 1B & 2B) were slightly better than the CR blends. However, after the TFOT the higher percentages (20 & 40_ CR) exhibited better BTS. Similar trends are evident in the Estimated Thermal Cracking Temperature (ETCT) on TFOT residue--which show lower ETCT (more resistant to theFmal cracking) for high _ CR blends.

The aging index increased with increased amounts of CR (Figure 4), however, per- cent of original penetration at 25C showed no significant change with increased CR (Table 1A & 2A). TFOT penetrations at 4C generally increased with increasing amounts of CR (Figure 5)uwhich is beneficial for low temperature properties of the pavement.

Based on binder evaluation of the two CRs in Arabian Heavy, there is little evidence of reduced performance. With the exception of spot test results, all Arabian Heavy-CR blends tested meet current AASHTOH-226 Table 2 requirements.

CALIFORNIA VALLEY

California Valley is recognized as an asphalt with high temperature suscepti- bility, and because of this is generally considered a marginal perfomer in areas with large seasonal temperature changes. It easily exceeds AASHTOt4-226 Table 1 requirements for temPerature susceptibility (minimum 40penetration at 25C and 1600 to 2400 poise at 60C), but fails to meet more stringent requirements found in Table 2. The California Valley AC-20 control has a 25C penetration of 50 and a 60C viscosity of 2059 poise, (Table 3A) and a BTS of -1.51 (Table 3B).

It can be seen that both CRs had a positive effect on the BTS (25C pen. & 60C visc.) for original properties and TFOT properties (Tables 3B & 4B). The 20 and 40%TJP and the 40_ Middle East CR blends improved the temperature susceptibility to the point that these blends meet AASHTOM-226 Table 2 (Tables 3A & 4A).

Low temperature properties were improved significantly with CR. For example, the ETCT for the control after TFOT was -21C while the 40_ TJP and Middle East CRS were -28 and -33C respectively (Table 3B & 4B).

The aging index did not increase with increased amounts of CR untii 40_ CR was used (Figure 6). Percent of original penetration at 25C did decrease with increasing CR, but this is probably a function of increased penetration (Table 3A & 4A). As previously discussed AASHTON-20 allows for a lower percent of original for a high penetration grade. Penetrations at 4C on the TFOT aged material in both cases increased with the higher amounts of conversion residue (Figure 7).

The improvement in BTS was primarily a function of the two CR crude sources as compared to the California Valley. However, Giavarini (ref 21) shows an increase in asphaltenes during the CR process. In this study six different residues from and their corresponding CRs were analyzed for asphaltenes. In all cases the • weight asphaltenes increased. The average asphaltene content for the six distilled residues was 11.0_, and for the corresponding CRs it was 15.0_ Two main reactions occur in visbreaking (ref 5 & 21). The primary reaction is the removal of Alkyl side chains (paraffins) from the molecules of the distilled residue. The secondary reaction is condensation of ring structures--increased molecular weight. Simpson et al (ref 22) found that the temperature suscepti- bility of an asphalt decreases with increasing molecular weight; and Corbett (ref 23) found that asphaltenes decrease the temperature susceptibility and are a desirable component of asphalt. Thus based on the above, a possible benefit from the CR process appears to be an improved BTS.

Based on binder evaluation of the two CRs in California Valley, there is strong evidence of improved performance (BTS). With the exception of some spot test results, all California Valley-OR blends tested meet current AASHTO M-226 Table I requirements; and the higher • of CR improved the resultant blends so they could meet Table 2.

BINDER EVALUATION IN BITUMINOUS MIXTURE

Three sources of aggregate were chosen from the SHRP Library in order to evaluate the effect of the various CR binders in the performance of mixtures in the presence of moisture. The aggregates selected for this phase of the evaluation were:

RA Lithonia Granite Vulcan Materials Co. Grayson, Georgia

RD Limestone Genstar Stone Product Frederick, Maryland

RL Golf Coast Gravel Fordyce Inc. Sullivan City, Texas

It was known from previous studies that the RA was prone to severe stripping, the RL to moderate stripping and the RD to little stripping.

Preliminary supplies of each aggregate were obtained from the SHRP Library and evaluated for gradation. Calculations indicated that satisfactory mixture

8 designs could not be prepared without additional fine aggregate. A supply of natural sand (FA-2) was obtained from SHRP source:

RF Glacial Gravel Vulcan Material Crystal Lake, Illinois

Marshall Mixture designs were prepared with each aggregate (RA, RD and RL) incorporating 301 of the natural sand (RF) using Arabian Heavy AC-20 (W 831). The designs were prepared in essential conformity with the procedures in the Asphalt Institute Manual MS-2. Optimum asphalt content was chosen at 4.0% air voids. This design data and blends are shown on Tables 5-7.

In order to evaluate the effect of the conversion residue to reduce moisture damage a series of fifty-four moisture induced evaluations were conducted. Each of the three aggregates were tested with two control asphalts AC-20 Arabian Heavy and AR-4000 California Valley. Each aggregate was also tested with blends of the above control asphalts and each conversion residue in concentrations of 5, 10, 20 and 40%.

The testing was conducted in accordance with ASTM Method D-4867. The data on these tests is summarized in Tables IC through 4C. Individual Data on each test is in the Appendix.

ARABIAN HEAVY

The test results for the ori9inal Arabian Heavy AC-20 indicate that all three aggregates have moisture damage potential (Table IC & 2C). The data indicates that the Georgia aggregate (RA) has the greatest damage potential as expected. However, the order of the Texas and Maryland aggregate was reversed from the expected performance. Both Tensile Strength Ratio (TSR) and the visual evaluation of stripping confirmed the ranking of the laboratory performance of the aggregates. The fact that the high percentage of natural sand (RF) from Illinois was needed for the mixture design could have confused the comparison of the laboratory versus field performance of the aggregates.

Georqia AQqregate (RA) - The test results for the Georgia Granite showed the greatest improvement of the study when the Arabian Heavy was blended with the Middle East CR. The TSR values increased from 20 with 0 percent CR to 69 with 40 percent CR. This is a statistically significant increase when testing precision reported in the ASTM Method is considered. When the Tia Juana Pesado CR was used, an increase in the TSR values was noted as the percentage of CR was increased. The blend of 40 percent Middle East CR with the Arabian Heavy brings the TSR values up to a marginal area. All other blends as well as the mixture without CR would need some additive to inhance the moisture damage potential of the mixtures. However, for all blends with this asphalt the TSR properties were equal to or better than the results on the mixtures without CR. The test results for the three aggregates and two CRs are shown on Figures 8&9. Visual evaluation confirmed that the stripping for the control and eight blends in this part of the study occurred in the coarse aggregate fraction. Maryland Limestone (RD) - The test results on Tables IC & 2C indicate that the 40 percent blends of both CRs brought the retained strengths for the Maryland limestone up to a value which would meet most state specifications. Both results are significantly different than the control results according to the ASTM precision statement.

In all cases, the CR blends were again equal to or better than the control tests with this aggregate. These results are in Figures 8&9.

Visual examinations of the moisture treated specimens again confirmed that the coarse aggregate fraction was the cause for the loss of strength.

Texas Chert (RL) - The test results given in Tables IC & 2C show a general increase in the TSR values for increased percentages of CR. These results are compared on Figures 8&9 for all three aggregates. None of the values are significantly different from the control tests. However, they are equal to and there appears to be a trend of better performance with more CR.

Visual evaluation of the moisture treated specimens confirmed that the strength loss was a result of coarse aggregate stripping.

Comments - The test results for the Arabian Heavy indicate in some cases a significant improvement in the moisture damage properties of the three aggregates studied. No detrimental performance was indicated with regard to moisture damage by this data. In all cases, the visual evaluation confirmed that the moisture damage occurred in the coarse aggregate fraction. This indicates that the natural sand (RF) used in the mix design did not have a detrimental effect on the performance of the aggregate blends. This is confirmed by the reasonable agreement between the laboratory data and the field performance history of the aggregates.

CALIFORNIA VALLEY

The moisture damage test results with the control asphalt indicate that the Georgia aggregate was approximately equal to if not better than the Maryland material and the Texas aggregate showed to be the worst. As previously indicated, this does not agree with previous field or laboratory experience. The Georgia material is a known stripper with TSR values expected to be in the 20 to 30 range if the material doesn't fall apart durin9 testing.

A further factor which confused this issue is the fact that none of the CR blends showed any significant benefit as experienced with the Arabian Heavy Study.

The visual evaluation of all the mixtures with the California Valley asphalt indicated that the vast majority of the stripping occurred in the fine aggregate fraction. This is totally different from the Arabian Heavy data and indicates that instead of evaluating three aggregates, only the natural sand RF from Illinois was studied.

Because of the concern over the major switch in data in this part of the study, an independent sample of California Valley asphalt was obtained (Not part of SHRP

10 MRL). The results of a new set of TSR tests on the Georgia aggregate are shown on Table 8. With this sample of asphalt, the TSR values decreased from 70 percent to the more common value of 28 percent with the coarse aggregate showing the stripping.

A study was undertaken to determine the differences in the asphalts which could cause such a major change. The results of a X-Ray fluorescence indicated that the SHRP MRL sample of California Valley asphalt contained 2400 parts per million of calcium compared to less than 50 parts per million for the check sample obtained independently. Other elements were present in virtually the same con- centrations in each sample. Following is the data obtained on the two California Valley asphalts.

SHRP Independent Element I Wt. % Wt. _T Al 0.06 0.08 Si 0.03 0.03 S 1.2 1.2 Ca < 50 PPM 0.24 Fe < 0.010 PPM < 0.010 PPM

Based on this information, it appears that a form of processing was used in the manufacturing of the SHRPMRL asphalt which introduced calcium into the material.

It appears that the calcium benefitted this asphalt such that when tested with the aggregates and CR in this study it masked the results. For this reason, the results of the California Valley asphalt moisture damage tests were not used to derive the conclusions to this study.

CONCLUSIONS

All the tests conducted in this study showed that conversion residue can be used in limited quantities with current asphalts. The data indicates a significant improvement in asphalt properties and moisture performance for a number of conditions. None of the tests indicated any adverse effect of the CR on the asphalt except for the spot test.

RECOMMENDATIONS

Based on the results of this study, it is recommended that several of the CR blends be shipped to other SHRP contractors for evaluation under the new binder tests being developed. If those results prove satisfactory, it is recommended that several test sections be built as part of the Long Term Pavement Performance Studies.

11 Appendix A

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36 CONSULTING TESTING

GENE ABSON, P.E. (1897-1963) _ RESEARCH

CONWAY C. BURTON,P.E. (CONSULTANT) RICHARD E. ROOT, P.E. 3360 COMMERCIAL AVENUEINORTHBROOK, ILLINOIS 60062 FOUNDED 1912 GEORGE J. GIROLIX,B.S EROL UNER, C.E.T. (708) 498-6400 FAX: (708) 498-7232 TABLE 5A

Report September 28, 1990 No. 006039

National Research Council Strategic Highway Research Program Attention: Mr. Robert R. Kelley 818 Connecticut Avenue, N.W. Washington, DC 20006

SHRP IDEAS - Georqia Granite (RA) Contract No. SHRP 87-ID020

Samples of aggregate were received from SHRP-Reference Laboratory for testing. A Marshall mix design was conducted in essential conformity with the procedures in the Asphalt Institute Manual MS-2.

Specimens were prepared from multiple batches and held at compaction temperature for 1.5 hours to simulate field conditions. Compaction was accomplished with a mechanical hammer and the maximum density was determined in accordance with ASTM Method D-2041.

The test data is summarized on the attached Report of Bituminous Mix Design and has been plotted on the Marshall data curves.

The following data summarizes the recommended mix design for the materials submitted.

Aqqreqate Proportions (Cold Feed):

Quantity Material Source

20_; No. 7 Georgia Granite (RA) 15_; No. 890 Georgia Granite (RA) 35_ No. 810 Georgia Granite (RA) 30_; FA-2 Crystal Lake (RF)

Optimum Asphalt Content for 75 Blow Desiqn: (Percent by Total Weight of Mix)

Grade Amount

AC-20 6.0

_-T,_....-.._,._ (W831 )

37

AS A MUTUAL PROTECTION TOCLIENTS, THE PUBLIC AND OURSELVES, ALL REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF OUR CLIENTS, AND AUTHORIZATION FOR PUBLICATION OF STATEMENTS, CONCLUSIONS OR EXTRACTS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUR WRITTEN APPROVAL. SAMPLES WILL BE DISPOSED OF 21 DAYS AFTER TESTING IS COMPLETED UNLESS OTHER ARRANGEMENTS ARE AGREEDTO IN WRITING. ALL TESTSARE CONDUCTED IN ACCORDANCE WITH THE LATEST ASTM OR AASHTO TEST METHODS WHERE APPLICABLE. TABLE _B

CHICAGO TESTING LABORATORY, INC

Report 006039

Marshall Properties at Optimum Asphalt Content:

Stability, at 140F, Ib .... 2770 Flow, at 14OF, 0.0_" . .... 10.5 Unit Weight, Ib/ft" 145.4

Voids Analysis, %: Air Voids ...... 4.0 Voids Mineral Aggregate . . 16.4 Voids Filled ...... 76

Job Mix Formula:

Sieve Size percent Pas_inR

3/4" ...... 100 1/2" ...... g5 3/8" ...... 67 No. 4 ...... _5 No. 8 ...... 54 NO. 16 ...... 42 No. 30 ...... 30 No. 50 ...... 15 No. 100 ...... 7 NO. 200 ...... 3.8

Asphalt Content, % ...... 6.0

RespectfulIy submitted,

CHICAGO TESTING LABORATORY, INC.

."....',._.,C.;.r_'[.!.iJ_'_L.._ Richard E. RooSt,PiE.

38 T%BI,F SC

2.50 ,,i ...... ' .... i , il " i , , ...... _;_ I _ ;_'!: if::; i : i - li 7i _i_i i : ;,:: 2.4o if!}17i: ;i ::::iiiTii';! ::ii ,;_ili i:;,i _ "'!:ii! i! _;_;71111:ii::'i: 8 !"_i!I_: _;; _ !i . :_ i:i:"i' !"ii 'i,i:'7 iif,i iii 'i _, ;...... ;,i { ii ,ii iiiii{i{i i <_ : :i!i iii: :i !lii_"i! ,_:i;iiii{ iT'!!!iiiir_ _"'_ii!!!iTiTi_ _ ' 'i i ,,"' _ _i,,...... ;, ....!!! i _ !_.,.4---.:. _-, ,!l!i, ,; :',i: . I--0 6 f' ' I "_ , _, 17: ..... '

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zoo I:_...... _ _' 1.i _...... ,,i_;:;, ...... i!i_, :!! 'i'i 0,,, _ '' _ " ' ,:;': :' '' 4.0 4.5 5.0 5.5 6.0 6.5 i.0 a_ 5.0 5.5 6.0 6.5 PERCENT ASPHALT CEMENT PERCENT ASPHALT CEMENT

, i _',i;;__' , " ; , i _L i,iiii!!i:, I ,* :i_!$I' ..... • - ' ..... ,,, 17 I , ' _0 ! ' i I !

,i": i : I 1 " ;'_ _,I, ,!t!! I-- iii:_i ;"'_-;-----_.,,,, ,_ . _ 'l 2500 !: ' :_-,-""-_;:: :_i . '.",';T'_,..i- , V,-...... _ _ : : ,,,.1 • "- ' ; _°_' : ' " ;_;_iil i _i : " 80 : _

, iII

- 2000 !::.,;:i:_,i.'.I i :: ....,!'.: r'._, _:.. : _. ,_.: 15 i<-- ! _' !! ;i :: i, , _ uJ" 70 rI ,, , ' _ ",: ' , i!' i,:,, ,;; I ii;! ' !':,i ' ,I ,i,,,i_ i!: "_ _i,;i;! .... i .... ;

1500 ..... i_;; :, ii,_{,!:i ; i'.._...... _ _.._' " '; ' " ': ...... : 14 !_I,.... , i,,...... !i ; i:['i 5> so ..;.;: ..', ": .... i _i_.i ii:,,_;,'!!'.!i i : ! i !i_i,;iii, :., . , , ,,

4.0 4.5 5.0 5.5 6.0 6.5 4.0 4.5 5.0 5.5 6.0 6.5 PERCENT ASPHALT CEMENT PERCENT ASPHALT CEMENT

25 '_:7i !''' i....i:_ i# i...... :.i

20 , :' I " "" ",i ;i';::::i BITUMINOUS MIXTURE DESIGN ' : :<:;ii_ By The MARSHALL METHOD tJ) ' L' " ,; .... i ': 006039 Date 9/ Oz 15 'i_i::; ':',, _,: '::.i_T, . !"i';:ii l_b. No. I 28/90 z t! !" ; i Materi-',ls Used

- _:,_..... _ ' Georgia Granite I lO _, , :, ;', +:. !:! " !!_,. o _ ! ': _ _!:...... 20% No. 7 i,I,. i i_':!i: _:; ;ii 'i ;il;i! :,' 15% No. 890 s " ' ' _.... _ !!_ 35% No. 810 !, !' i ,II; '!, " _ ,_ , :i : ',_'!! 30 No. FA-2

o , ' ' CHICAGO TESTING LABORATORY. INC. 4.0 4.5 5.0 5.5 6.0 6.5 33_ COMMERCIAL AVENUE PERCENT ASPHALT CEMENT NORTHBROOK. ILLINOIS oo662 39 TABLE 5D

REPORT OF BITUMINOUS MIX DESIGN LAB. NO. 006039 DATE 9/28/90

TO: SHRP Ideas - Georgia Granite (RA) TYPE: Surface

MATERIALS SUBMITTED CTL No Agg Source 004102 No. 7 Georgia Granite (RA) 004104 890 Georgia Granite (RA) 004103 810 Georgia Granite (RA) 007131 FA 2 Crystal Lake, Illinois (RF)

AGGREGATE GRADATION - PERCENT PASSING No. 7 890 810 FA 2 Blend Sieve

3/4" 100,0 100.0 1OO.0 100.0 100.0 1/2" 75.7 100,0 1OO.0 100.0 95.1 3/8" 37.0 97,5 100.0 100.0 87.0 No 4 3.4 20.0 90.7 99.8 65.4 No 8 2.0 2,6 77.2 85.9 53,6 No 16 1,7 1.6 65.3 62.1 42.1 No 30 1.4 1,2 50.2 39.1 29.8 No 50 1,0 0.7 32.1 11.0 14.8 No 100 0.7 0.5 18.0 2.1 7.1 No 200 0.4 0.2 9.6 1,2 3.8

Agg BSG 2.627 2.613 2.634 2.629 2.628

AGGREGATE BLEND Percent 20.0 15.0 35.0 30.0 100.0

BITUMEN DATA Type : AC-20 Source: '004208 SG :1.034

MARSHALL MIXTURE DATA TEMP. MIX- 315 COMP.- 290 BLOWS- 75

Bitumen BSG MSG Voids VMA Vf Flow Stab 4.5 2.291 2.488 7.9 16.7 52.8 9.7 2620 5.0 2.306 2.469 6.6 16.6 60.2 9.8 2595 5.5 2.318 2.451 5.4 16.6 67.3 10.2 2800 6.0 2.339 2.434 3.9 16.3 76.2 10.2 2820 6.5 2.344 2.416 3.0 16.6 82.0 10.8 2470

Agg ESG 2.664 Asphalt Abs, % 0.5

COMMENTS:

40 CHICAGO TESTING LABORATORY, INC. TABLE 6A

Report September 29, 1990 No. 006040

National Research Council Strategic Highway Research Program Attention: Mr. Robert R. Kelley 818 Connecticut Avenue, N.W. Washington, DC 20006

SHRP IDEAS - Maryland Limestone (RD) Contract No. SHRP 87-ID020

Samples of aggregate were received from SHRP-Reference Laboratory for testing. A Marshall mix design was conducted in essential conformity with the procedures in the Asphalt Institute Manual MS-2.

Specimens were prepared from multiple batches and held at compaction temperature for 1.5 hours to simulate field conditions. Compaction was accomplished with a mechanical hammer and the maximum density was determined in accordance with ASTM Method D-2041.

The test data is summarized on the attached Report of Bituminous Mix Design and has been plotted on the Marshall data curves.

The following data summarizes the recommended mix design for the materials submitted.

Aqqreqate Proportions (Cold Feed):

quantity Material Source

15% No. 7 Maryland Limestone (RD) 10% I/2-4 Maryland Limestone (RD) 10% Birdeye Maryland Limestone (RD) 35% 10 Sceenin9 Maryland Limestone (RD) 30% FA-2 Crystal Lake (RF)

Optimum Asphalt Content for 75 Blow Design: (Percent by Total Weight of Mix)

Grade Amount

AC-20 5.5 (ws31)

41 TABLE 6B

CHICAGO TESTING LABORATORY, INC

Report 006040

Marshall Properties at Optimum Asphalt Content:

Stability, at 140F, Ib .... 2550 Flow, at 140F, 0.0_" . .... 10.8 Unit Weight, Ib/ft" . 149.8

Voids Analysis, _: Air Voids ...... 4.0 Voids Mineral Aggregate . . 15.0 Voids Filled ...... 75

Job Mix Formula:

Sieve Size Percent Passinq

3/4" ...... 100 i/2" ...... gs 3/8" ...... 93 No. 4 ...... 73 No. 8 ...... 52 No. 16 ...... 35 No. 30 ...... 22 No. 50 ...... 10 No. 100 ...... 6 No. 200 ...... 4.B

Asphalt Content, % ...... 5.5

Respectfu IIy submitted,

CHICAGO TESTING LABORATORY, INC.

Richard E. Root, P.E.

42 TABLE 6C

t50 10

,;_...... i .... !; :::_;,:_ " :_= !"!i i!t' '" ' ';!"

i _,, x Jl

, ,, _ ,,_, ,, ,_ t,i ' _ _..:"" ...... _,: ..... !!t,_ _' ii!iii!ii:! i ,,i i '_ J ,q 2.30 ii il i i:{! i : ! I ...... • ! ,

;!i: ,::' _ii:: ii! _i_i:i...... '_: !iiii;!!; " ::, :_: _'_:: iii!!{: .i; ;;I:::

2.10 !!!' ' i! i: ;i; _ ;iiil;' ': :i;;;l; _ o.. 2 il t: ;i:! I :I,, . _"_.;

i_i{'!ii!,, _" ; :i:i!!;:!_!;ii, , II :i .;:;,: ,,,i_;_;_,,_,:,::, ...... ,,;, .... : .... , .... :; • ' " ..... iiii!!:': I, i, 2.00 ...... i!!!: ;:i :_! { _-:!i,!i;, :; !"_:; :_,_,_,i: 0 .... ',; ...... ' 4.0 4.5 5.0 5.5 6.0 6.5 4.0 4.5 5.0 5.5 6.0 6.5 PERCENT ASPHALT CEMENT PERCENT ASPHALT CEMENT

3500 too ;ii,i,;,,!I_:_,'''_;_,,:'r',:_:,'::'':',i:i'_";i;_i'::__;,iiii,i I ii__:""...... _; '_'''i!;!'':' :',' :, : , • ,,if, , , . ,i', !t,, .... ,ii,, 3000 :!: _;'=l'i ; ! ' ' ' ). ': !:_,;_, _ I ; ..... ;_: ",!I _ ' '', i: r, _, .= 90 ,t ' li' " I ' ,' .' '_i i! !i !:1'...... Iii 'I > i' ! 'I , ii' "1_ ; i".i : ii,:i i i _ ,_ , -- ; ' !I; ' _ :i _: i • '.,I ,' ;,,',', ,,,', '. ', ,!',_I, _ ,:,,' ;: ,l] I_,- ,

>- ' • ' " '" "

( _;_I:[ ' .::Ii : ;',: : :! ! !T _ 70 - ,x I I :,,_,.,, ,,_ :i:'i: ,::,,: !_I ' "" ,"" ':1 '_; _ '" 1500 ',!'i':,! '" ' ::' 'i ,-, ,!,,:, .;.. ,,' , , ,, ' i, I " I' " " _:' "' ',';:I',!;! '_ "

1000 ',:,, ], , .....': , , : : ' 50 , i , ' ': 4.0 4.5 5.0 5.5 6.0 6.5 4.0 4.5 5.0 5.5 6.0 6.5 PERCENT ASPHALT CEMENT PERCENT ASPHALT CEMENT

25 i ::_ ; ' :;_i:!! =_ ', "'!!_i

_: ' ,ii!i!i' ...... iii_i' , ,,_ i_iii 20 •' , , , _;, i , ii BITUMINOUS MIXTURE DESIGN :: :;i :_ ;!':_ i By The MARSHALL METHOD -,- ...... 9/29/90 O'" 15 :'" ' I' [; I , ; }!: !. iiiii_i_, Lab.No. 006040 IDate !: : ,,:. , ,. ;:: . ;i:,_-": Materials Used

I 10 "." . i ':: _ : i;ii:, 15% NO. 7 o _; :: ',;_i: !, ':_ : iii,: _ -;_ .i_i:i:,_ 10% 1/2-4 ,[ i, .: ::-,. 10% Birdeve

,:; i .... ] ,,I ' ! ; _ ',',', , 35% 10 Screening ...... ;,,, ,, 50% FA-2 I _ ' " I '' O: _ I ;' ' " ' ;' CHICAGO TESTING LABORATORY. INC. 4.0 4.5 5.0 5.5 6.0 6.5 3300 COMMERCIAL AVENUE PERCENT ASPHALT CEMENT NORTHBROOK L,LINOIS __062 43 TABLE 6D REPORT OF BITUMINOUS h_IX DESIGN LAB. NO. 6040 DATE 9/29/90

TO: SHRP Icleas - Maryland Limestone (RD) TYPE: Surface

MATERIALS SUBMITTED CTL No Agg Source 4111 No. 7 Maryland Limestone (RD) 4109 1/2-4 Maryland Limestone (RD) 4107 Birdeye Maryland Limestone (RD) 4.112 10 Scrn Maryland Limestone (RD) 7131 FA-2 Crystal Lake, Illinois (RF)

AGGREGATE GRADATION- PERCENT PASSING No. 7 1/2-4 Bird 10 Scrn FA 2 Blend Sieve 3/4" 10,3.0 100.0 100.0 100.0 100.0 100.0 1/2" 83.3 100.0 100.0 100.0 100.0 98.4 3/8" 57.6 91.1 100.0 100.0 100.0 92.8 No 4 8.5 14.0 67.6 95.7 99.8 72.9 No 8 2.2 3.0 22.7 68.0 85.9 52.5 No 16 1.3 1.2 6.6 43.1 62.1 34.7 No 30 :.1 1.0 4.0 28.0 39.1 22.2 NO 50 1.1 0.8 3.1 19.0 11.0 10.5 No 100 1.0 0.7 2.7 14.0 2.1 6.0 No 200 0.9 0.7 2.6 11.4 1.2 4.8

Ago BSG 2.710 2.691 2.699 2,683 2.629 2,673

AGGREGATE BLEND Percent 15.0 10.0 10.0 35.0 30.0 100.0

BITUMEN DATA Type : AC-20 Source: '004208 SG :1.034

MARSHALL MIXTURE DATA TEMP. MIX- 315 COMP.- 290 BLOWS- 75

Bitumen BSG MSG Voi ds VMA Vf Flow Stab 4.5 2.273 2.537 ,6.5 15.2 57.4 9.7 2625 5.0 2.387 2.518 5.2 15.2 65.6 10.3 2490 5.5 2.410 2,499 3.6 14.8 75.8 10.2 2590 6.0 2.414 2.481 2.7 15.1 82.2 12.2 2370 6.5 2,420 2.462 1.7 15.3 88.8 17.0 2050

Ag9 ESG 2.724 Asphalt Abs, • 0.7

COMMENTS:

44 CONSULTING TESTING

GENE ARSON, P.E. (1887-1963) _ RESEARCH

CONWAY C. BURTON, P,E. (CONSULTANT) RICHARDE.ROOT,P.E. 3360COMMERCIALAVENUE/NORTHBROOK,ILLINOIS60062 FOUNDED1912 GEORGE J. GIROUX, B.S. WAREROL UNERP, C.E.T.ADPRRE,,,,,2'=, (708) 498-6400 FAX:VN(708) VD498-7232[ ® B @O

TABLE 7A

Report February 5, 1991 No. 006041-A

National Research Council Strategic Highway Research Program Attention: Mr. Robert R. Kelley 818 Connecticut Avenue, N.W. Washington, DC 20006

SHRP IDEAS - Texas Chert (RL) Contract No, SHRP 89-ID020

Samples of aggregate were received from SHRP-Reference Laboratory for testing. A Marshall mix design was conducted in essential conformity with the procedures in the Asphalt Institute Manual MS-2.

Specimens were prepared from multiple batches and held at compaction temperature for 1.5 hours to simulate field conditions. Compaction was accomplished with a mechanical hammer and the maximum density was determined in accordance with ASTM Method i)-2041.

The test data is summarized on the attached Report of Bituminous Mix Design and has been plotted on the Marshall data curves.

The following data summarizes the recommended mix design for the materials submitted.

Aqqreqate Proportions (Cold F¢ed):

Quantity Haterial Source 301; No. 4 Texas Chert (RL) 15Z No. 6 Texas Chert (RL) 24_ 8-200 Texas Chert (RL) 304 FA-2 Crystal Lake (RF) 11; Dust Texas Chert (RL)

Optimum Asphalt Content for 75 Blow Desi,qn: (Percent by Total Weight of Mix)

S}_: Grade Nnount _ AC-20 6.2 _; _"_ (we31) 4S

AS k MUTUAL PROTECTION TO CLIENTS, THE PUBLIC AND OURSELVES, ALL REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF OUR CLIENTS, AND AUTHORIZATION FOR PUBLICATION OF STATEMENTS, CONCLUSIONS OR EXTRACTS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUR WRITrEN APPROVAL. SAMPLES WILL BE DISPOSED OF 21 DAYS AFTER TESTING IS COMPLETED UNLESS OTHER ARRANGEMENTS ARE AGREED TO IN WRITING, ALL TESTS ARE CONDUCTED IN ACCORDANCE WITH THE LATEST ASTM OR AASHTO TEST METHODS WHERE APPLICABLE. TABLE 7B

CHICAGO TESTING LABORATORY, INC

Report 006041-A

Marshall Properties at Optimum Asphalt Content:

Stability, at 140F, lb .... 1860 Flow, at 140F, 0.01" . .... 9.1 Unit Weight, Ib/ft3 143.3

Voids Analysis, ¢: Air Voids ...... 4.0 Voids Mineral Aggregate . . . 16.0 Voids Filled ...... 75

Job Mix Formula:

Sieve Size Percent PassinR

1/2" ...... 100 3/8" ...... 90 No. 4 ...... 67 No. 8 ...... 51 No. 16 ...... 38 No. 30 ...... 28 No. 50 ...... 17 No. 100 ...... 4 No. 200 ...... 2.4

Asphalt Content, ¢ ...... 6.2

Respectfu 1ly submitted,

CHICAGO TESTING LABORATORY, INC.

Richard E. Root, P.E.

46 • !!,

8 ;:"

iii::

;i_[i ill_. m w iiii! _10 2 i!ii_!!!:: !;iii !i: " _00 O 5.0 S.5 6.0 6_5 7.0 7.5 5.0 5.5 6.0 6.5 7.0 7.5 PERCENT ASPHALT CEMENT PERCENT ASPHALT CEMENT

_oo 18

_ -,t-

1000 wo 70 zu, p- .,J

U_

r_ ¢

0 5.0 5.5 6.0 6.5 7._0 7_5 5.0 5.5 6.0 6.5 7.0 7.5 PERCENT ASPHALT CEMENT PERCENT ASPHALT CEMENT

25

20 BITUMINOUS MIXTURE DESIGN By The MARSHALL METHOD

IJJ •_- Lab. No. 006041-A Date 2/5/91 o 15 MateriaLs Used Z 30% No. 4 (RL) _- 15% No. 6 (RL) I lo 24% 8-200 (RL) 30% FA-2 (RF) .J _- 1% Dust 5 AC-20

0 CHICAGO TESTING LABORATORY, INC.

s.o J.o NORTHBROOK. ILLINOISAvENuE60062 47 TABLE 7D REPORT OF BITUMINOUS MIX DESIGN LAB. NO. 306041A DATE 1/22/91

TO: SHRP Ideas - Texas Chert (RL) TYPE: Surface

MATERIALS SUBMITTED CTL No Agg Source 4115 No. 4 Texas Chert (RL) 4116 No. 6 Texas Chert (RL) 2109 8-200 Texas Chert (RL) 7131 FA-2 Crystal Lake, Illinois (RF) 4117 Dust Screened from -200 Material

AGGREGATE GRADATION - PERCENT PASSING No. 4 No, 6 8-200 FA-2 Dust Blend Sieve

3/4" 100.0 100.0 100,0 100.0 100,0 100.0 1/2" 99.4 100.0 100.0 100.0 100.0 99,8 3/8" 67.0 99.8 100.0 100.0 100.0 90.1 No 4 1.7 79.1 99.9 99.8 100,0 67,3 No 8 0.3 7.8 94.5 85.9 100.0 50.7 No 16 0.2 0,6 76.4 62.1 100.0 38.1 No 30 0,1 0.2 65.6 39.1 100,0 28.5 No 50 0.1 0.1 51,7 11.0 100.0 16,8 No 100 0.1 0.1 10.9 2.1 100,0 4.3 No 200 0.0 0.0 4.3 1.2 100.0 2.4

Agg BSG 2.597 2.578 2.485 2.629 2.562 2,575

AGGREGATE BLEND Percent 30.0 15.0 24.0 30.0 1.0 100.0

BITUMEN DATA Type : AC-20 Source: 004208 SG :1.034

MARSHALL MIXTURE DATA TEMP. MIX- 315 COMP.- 290 BLOWS- 75

Bitumen BSG MSG Voids VNA Vf Flow Stab 5.0 2.275 2.447 7.0 16.1 56.2 8.7 1850 5.5 2.283 2.430 6.0 16.2 62.8 9.7 1800 6.0 2.295 2.413 4.9 16.2 70.0 8.8 1840 6.5 2.311 2.396 3.5 16.1 78.1 9.0 1870 7.0 2.316 2.379 2.6 16.4 83.9 10.2 1710

A99 ESG 2.637 Asphalt Abs, % 0.9

COMMENTS:

CM!CAGO TESTING LABORATORY, INC. 48 ID

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103 References

1. Shell International Company Limited. The Petroleum Handbook. Fifth edition. 1966.

2. Oliensis, G. American Society of Testing Materials. Proceedings 33. 1933.

3. The Asphalt Institute, "State Specifications of Asphalt." July 1987.

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