bluuebunny/crossref_metadata_2025 huggingface dataset:
Materials for Use at Liquid Hydrogen Temperature
Authors: Belton John H. , Godby Larry L. , Taft Barrett L.
Published: August 2009

Low-temperature tensile properties and average coefficients of linear expansion from low to ambient temperature were obtained for materials applicable to rocket engines including aluminum-, nickel-, iron-, copper- and titanium-base alloys and plastics. Procedures and techniques for tension and expansion coefficient testing at liquid hydrogen temperature (−423 F) and descriptions of testing chambers are given. Some alloys tested showed very high tensile strength while maintaining good ductility at liquid hydrogen temperature. Alloys considered suitable for use with liquid hydrogen include wrought and cast aluminum, nickel, copper and 9310 and A 286 steel. In general, coefficients of linear expansion decreased as temperatures approached that of liquid hydrogen.
Effect of Zerolling on Properties of Modified Type 347 Stainless Steel
Authors: Mayne Charles R.
Published: August 2009

Chromium-nickel stainless steels have excellent properties at subzero temperatures. All metallic materials increase in strength as temperature is reduced below 0 F, but unfortunately the increase in strength is often accomplished by decreased ductility and increased brittleness. However, the annealed 18-8 alloys, as shown by Colbeck, McGillivray, and Manning (1), Rosenberg (2), McAdam, Geil, and Cromwell (3), and many other investigators, show a great increase in tensile strength at subzero temperatures without any great loss in ductility, reduction of area, or impact resistance. Krivobok and Talbot (4) and Zambrow and Fontana (5) showed that 18-8 alloys rolled to high tensile strength at room temperature exhibited much better ductility at temperatures down to −320 F than at room temperature, and at the same time the tensile strengths were increased. Zambrow and Fontana also investigated the effect of temperature on the impact strength. They found that at temperatures down to −423 F, the lowest temperature investigated, cold-rolled type 304 stainless steel had better impact strength than at room temperature. Krivobok and Talbot (4) and Ziegler and Brace (6) showed that working stainless steels at subzero temperatures resulted in greatly increased tensile strengths. If these “zerolled” stainless steels are heated to temperatures up to 800 F, additional strengthening takes place. The increase was particularly noticeable in type 347 stainless steel. Thus it was decided to investigate these effects further.
Low-Temperature Properties of Cold-Rolled AISI Types 301, 302, 304ELC, and 310 Stainless Steel Sheet
Authors: Watson James F. , Christian J. L.
Published: August 2009

The cold-rolled austenitic stainless steels have assumed an important position in missile and space vehicle applications where they are used as skins and other highly stressed structural members at temperatures ranging down to −423 F (the boiling point of hydrogen). The critical nature of structural weight and pressure integrity in pressurized cryogenic propellant tanks in this application requires a material having an optimum combination of high strength-density ratio, weldability, and resistance to brittle fracture at cryogenic temperatures, as well as adequate formability and corrosion resistance. The AISI type 300 series austenitic stainless steels are used for this type of application because of their excellent weldability and toughness at low temperature and their moderately high strength-density ratios which improve markedly at lower temperatures. In this investigation, the mechanical properties of a series of cold-rolled austenitic stainless steels were determined at 78, −100, −320, and −423 F. The alloys were studied in a variety of cold-worked tempers in thicknesses varying between 0.013 and 0.032 in. These alloys were subjected to tension tests in both smooth and notched (stress concentration factor, Kt = 6.3) configurations to provide values of yield and tensile strength, elongation, notched-unnotched tensile ratios in the base metal, and tensile strength and elongation in heliarc butt welded joints. The notched tension tests were included in this study to evaluate toughness which is a measure of resistance to brittle failure. Toughness is a property of vital importance in missile design because these missile structures are subject to shock-type loads which occur during hydraulic hammering, vibration due to rocket engine firing, and action of quick closing valves, and will contain built-in stress concentrations of varying degrees of intensity due to welding defects, tool marks, assembly eccentricities, and random defects in the metal. These conditions all favor brittle failure, and become even more severe at low temperature in that brittle fracture is more prone to occur at reduced temperatures.
An Evaluation of Compression Testing Techniques of Sheet Materials at Elevated Temperatures
Authors: Gerard George
Published: August 2009

This program was conducted in order to assess the accuracy of several compression testing techniques of sheet materials at elevated temperatures. The information obtained on the various techniques under relatively controlled conditions was used as a guide in establishing uniform compression testing procedures for the Titanium Sheet Rolling Program.
Rapid-Rate Compression Testing of Sheet Materials at High Temperatures
Authors: Bernett E. C. , Gerberich W. W.
Published: August 2009

This paper describes the test equipment developed and the procedures used to evaluate structural sheet material compression properties at preselected constant strain rates or loads. Electrical self-resistance was used to achieve a rapid heating rate of 200 F per sec. Four materials were tested at maximum temperatures which ranged from 600 F for an aluminum alloy to 2000 F for a Ni-Cr-Co iron-base alloy. Tests at 0.1,0.001, and 0.00001 in. per in. per sec showed that strain rate has a major effect on the measured strength, especially at the high temperatures. The tests, under conditions of constant temperature and constant compression stress, showed that creep deformation can be a critical factor even when the time involved is on the order of a few seconds or less. The theoretical and practical aspects of rapid-rate compression testing are presented, and suggestions are made regarding possible modifications of the equipment which would improve the over-all capabilities.
Compression and Buckling Characteristics of Annealed and Aged Inconel 718 Nickel-Chromium Alloy at Temperatures up to 1400 F
Authors: Dubuc J. , Welter G.
Published: August 2009

A special fixture developed at Ecole Polytechnique was used to carry out compression tests on strips of sheet material at room and high temperatures up to 1400 F, to determine the stress-strain diagram in compression of annealed and aged Inconel 718 nickel-chromium alloy. Buckling tests at room and high temperatures were also carried out on columns of the same material and of various slenderness ratios, using specially developed pin-ended supports enabling lateral displacement under load of one end of a column; this feature together with a precise centering technique permitted keeping a column well centered during a buckling test. The theoretical relationship between buckling stress and slenderness ratio for columns made of this material was calculated by Euler's formula using the tangent modulus determined from the experimental compression stress-strain diagrams. Experimental buckling stresses of columns were found to agree well with the calculated values. Thus, not only is the experimental relationship established between buckling stress and slenderness ratio for columns of annealed and aged Inconel 718 nickel-chromium alloy, but it is also shown that the buckling behavior of such columns can be accurately predicted from the compression stress-strain diagrams of the material.
Evaluation of a System for Compression Testing of Sheet Materials at Elevated Temperatures
Authors: Breindel W. W. , Carlson R. L. , Holden F. C.
Published: August 2009

A critical evaluation is presented of a system that has been used to obtain compression stress-strain data for sheet materials at elevated temperatures. Descriptions of the supporting apparatus for the specimen, the method of heating, specimen design, and the method of strain measurement are presented. Particular emphasis is centered on the effect of lateral support afforded the specimen by the fixture. Illustrations showing the effect of modifications in the method of support are included, as well as some typical experimental results.
The Need for Better Simulated Service Tests for Packaging
Authors: Jordan C. A.
Published: August 2009

Environmental hazards imposed on packages in the process of moving goods from producer to consumer may have damaging effects on improperly designed packages or contents. Current tests and procedures for evaluating packages and packaging materials in the laboratory attempt to simulate these environmental hazards, but the degree of correlation between these tests and the actual service hazards has not been established. The fact that the mechanical hazards involve dynamic forces has been a deterrent to their proper evaluation and to their proper simulation in the package-testing laboratory. Only in recent years has suitable instrumentation for studying the response of packages, package components, and contents to dynamic forces become available. An instrument capable of producing a faithful and complete record of the dynamic loads imposed on a given package during a specific delivery cycle has yet to be developed. Given adequate data on the nature and extent of dynamic forces imposed upon packages in service, the application of statistical methods will provide a sound basis for the establishment of realistic simulated service tests.
Rail-Car Impact Simulator
Authors: Patterson D. , Lantos P. R.
Published: August 2009

A new tester has been developed to measure the effects of impacts encountered by containers in rail-car shipment. Typical results for several constructions of industrial bagging materials are shown. Correlation with actual controlled rail-car impact tests has been demonstrated and statistically verified.
The Development of the Zircaloys
Authors: Kass Stanley
Published: August 2009

The experimental work leading to the development of Zircaloys -1, -2, -3, and -4 is reviewed. The corrosion properties of Zircaloys -2 and -4 in high temperature water and steam, and the effects of composition, heat treatment, and water chemistry upon oxide film formation and hydrogen absorption during corrosion are also discussed.
Effect of Fluoride Ions on the Aqueous Corrosion of Zirconium Alloys
Authors: Berry Warren E.
Published: August 2009

A review has been made of the effects of fluoride ions on the corrosion behavior of zirconium alloys in high-temperature water. Corrosion was found to occur as the result of contamination of the water or the zirconium surface. A major source of fluorides is undue delay in rinsing the HF-HNO3 pickling solution during surface preparation. The oxide on corrosion-resistant material has been found to contain up to 7600 ppm fluoride from this source. The threshold concentration of fluoride in the oxide film which produces poor corrosion resistance ranges from 8500 to 17,000 ppm. Accelerated corrosion from fluorides in water at 300 to 360 C occurs at about 100 ppm, although increased corrosion has been reported at 10 ppm fluoride in water at 300 C. Fluorocarbon plastics degrade and contribute fluorides to the high-temperature water or to the alloy surface when in direct contact with zirconium. Chlorides (1 to 10,000 ppm) and iodides (1270 ppm) do not adversely affect the corrosion behavior of zirconium alloys in water at 360 C. The mechanism of corrosion is not well understood but apparently is related to the formation of insoluble zirconium oxyfluorides during pickling and during exposure to fluoride-contaminated water.
Relationships Between Microstructure and Toughness in Quenched and Tempered Ultrahlgh-Strength Steels
Authors: Baker A. J. , Lauta F. J. , Wei R. P.
Published: August 2009

An investigation was made of a number of 0.30 and 0.40 per cent carbon alloy steels to determine the relationships between their fracture toughness properties and their internal microstructures. The plane-strain fracture toughness of the steels was measured after tempering quenched material in the temperature range 300 to 1100 F. A thin section transmission electron microscopy study was carried out on the tempered materials. From the fracture toughness studies it was concluded that all the materials behaved similarly and that alloying elements (carbon and silicon) had little influence on the general relationship between tensile strength and toughness in these fully hardenable steels. It was found that the fracture toughness remained low at low tempering temperatures but improved rapidly once a critical tempering temperature, characteristic of the particular steel, was reached. The microscopy study showed that major microstructural changes occurred in the tempering range where the rapid increase in toughness was observed. At low tempering temperatures the defect structure of the as-quenched martensite remained unchanged, and continuous films of carbide were formed in the boundaries of the martensite. In the critical tempering range the carbide films were spheroidized and the defect structure of the matrix removed or modified by recovery processes. On the basis of these observations, it was concluded that the low fracture toughness of the steels in a lightly tempered condition was due to their high defect densities and the presence of carbide films at boundaries. Only when these features were removed or modified did toughness increase.
Relationships Between Structure and Properties in the 9Ni-4Co Alloy System
Authors: Pascover J. S. , Matas S. J.
Published: August 2009

The effects of alloy content and heat treatment on the strength and toughness of 9Ni-4Co alloy steels are discussed in detail. The strength was determined with standard tension specimens, while toughness was evaluated with various accepted, sharply notched specimen types. Of the alloying elements used, carbon acted as the strongest embrittler but was necessary as a strengthener. Silicon and the carbide-forming elements decreased toughness, particularly at higher carbon contents. Hence, the use of silicon at other than residual levels was undesirable. The addition of carbide-forming elements in appreciable amounts needed careful consideration. Nickel was used in substantial amounts to improve toughness, while cobalt was added to inhibit retained austenite formation consequent upon the high nickel content. Cobalt enhanced self-tempering effects, particularly for the lower carbon varieties. Heat treatment strongly influenced the properties as a result of the attendant changes in the microstructure. Isothermal transformation to lower bainite enhanced toughness in the 0.45%C, 9%Ni-4% Co high performance (HP) 9-4-45 steel. The toughness was superior to that of tempered martensite at equivalent strengths. The properties of upper bainite were not as attractive as those of lower bainite. Mixed structures composed of bainite and martensite lowered toughness. The two commercial grades of the 9Ni-4Co alloy system, HP 9-4-25 and HP 9-4-45, had a better combination of strength and toughness than other carbon-strengthened steels. The self-tempering characteristics of the HP 9-4-25 grade and its inherent toughness contributed to high joint efficiences and formability in the as-welded condition. No post-heat treatment of the welded joint was required.
The Metallurgy and Properties of Cold-Rolled Am-350 and Am-355 Steels
Authors: McCunn T. H. , Aggen G. N. , Lula R. A.
Published: August 2009

AM-350 and AM-355 are controlled-transformation precipitation-hardening steels. AM-350 is more familiarly known in sheet and AM-355 in bar form where hardening is produced by heat treatments alone. Annealed at 1900 F, the materials are essentially austenitic at room temperature, but the austenite is very unstable. By cold deformation, a substantial amount of martensite is formed. The mechanical properties of cold-rolled products can be controlled over a wide range and vary as functions of per cent deformation, amount of martensite produced, and tempering treatment. The mechanical properties of these materials are extremely interesting from an engineering point of view. Higher strength with better toughness can be attained than with Type 301, which is the stainless steel generally used in the cold-rolled condition. This paper deals with the metallurgy and properties of cold-rolled AM-350 and AM-355. The mechanical properties are shown as functions of the amount of deformation, deformation temperature, and prior annealing temperature. More detailed mechanical properties of AM-350 and AM-355 CRT (20 to 30 per cent reduction) are given including toughness studies. AM-350 in particular has been evaluated for the supersonic transport and appears to meet the stringent requirements for this application.
Fracture Micromechanics in High-Strength Steels
Authors: Banerjee Bani R.
Published: August 2009

Because tempered martensites provide some of the most desirable combinations of strength and ductility, a study was made of secondary-hardening steels—Type H-11 (Crucible 218) and Type 422, and a martensitic-hardening low-alloy high-strength steel, Type 4340—to relate fine structural aspects to strength and fracture properties. The fracture process was shown to consist of many discontinuous crack initiation, coalescence, and propagation steps merging together to produce the macroscopic fracture front. The observed large scatter in fracture toughness of air-melt 4340 in the 500-F embrittlement region was explained in terms of the high sensitivity of the fracture-toughness test to structural discontinuities at inclusion-matrix interfaces in a deformation limited matrix. Such effects were absent in vacuum-melted 4340 steels. Tempering the two secondary hardening steels at temperatures well below the secondary hardening region produced an optimum combination of strength and toughness. A fourfold toughness benefit in 422 and a substantial benefit in 218 were thus demonstrated without loss of yield strength. Tempered-martensite embrittlement, 500 F, and temper brittleness, 900 to 1000 F, were explained in terms of a unified mechanistic concept involving precipitation locking of dislocation intersections and jogs, along with high dislocation densities during carbide re-solution and reprecipitation steps.
Ausform Fabrication and Properties of High-Strength Alloy Steel
Authors: Gerberich W. W. , Williams A. J. , Martin C. F. , Heise R. E.
Published: August 2009

The Ausform process has been developed for production applications to the point that the strength, ductility, and toughness of commercially available materials are improved by simply altering the order of conventional metal processing. Shear spinning is being used for Ausform fabrication of tubular components such as missile cases with electron-beam welding being utilized to girth weld head closures on finished cases. Electron-beam welding of steels in the Ausformstrengthened condition proved successful with joint efficiencies of 90 per cent obtained. In addition to the investigation of fabrication techniques, a detailed study of the crack propagation characteristics of ausformed steel is presented. A considerable amount of fracture toughness data obtained from longitudinally rolled specimens indicate that, for a commensurate yield strength, the toughness of the ausformed steel is much greater than the corresponding conventionally-treated material. For example, fracture toughness values well over 200 ksi √in. were attained for 250 ksi yield strength materials obtained by ausforming both D6AC and a low-carbon modified H-11. Charpy V-notch impact data give similar results for both closed die and high-energy-rate forgings made of low-alloy steels. With proper processing and alloying, toughness to strength ratios greater than that obtainable with maraging steels is possible.
Thermomechanical Treatments Applied to Ultrahigh-Strength Bainites
Authors: Kalish D. , Kulin S. A. , Cohen M.
Published: August 2009

The mechanical properties of H11 and AISI 4350 steels were determined for a series of bainites formed from both deformed and undeformed austenites. These bainites were also subjected to subsequent straining and tempering treatments. Similar thermomechanical treatments involving martensite as the essential transformation product were included for comparison purposes. Fifty per cent austenite deformation in H11 results in considerable strengthening of the subsequently formed bainite. H11 in the bainitic condition, formed from either deformed or undeformed austenite, is strongly affected by refrigeration in liquid nitrogen, owing to conversion of retained austenite when tempering temperatures below 1000 F are employed. In both cases, a large secondary strengthening is observed on tempering between 1000 and 1100 F. This results in higher strengths and equivalent ductilities as compared to the correspondingly treated martensites. Austenite deformation in 4350 has little effect on the strength of the subsequently formed bainite, although such deformation does enhance the strength of martensite. H11 and 4350 bainites and martensites exhibit a large response to strain-tempering treatments. For both steels, small deformations (up to 3 per cent) produce large strengthening effects. Yield strengths close to 400,000 psi have been obtained by the application of strain-tempering treatments (50 per cent deformation) to both H11 martensite and bainite. Increasing the carbon content in 43XX steels enhances the strengthening response to strain-tempering. The increments in strength developed by deformation processes, both before and after transformation to either bainite or martensite, are found to be approximately additive when the individual processes are combined.
X-Ray Spectrochemical Analysis of Materials: Cement and Dental Alloys
Authors: Bean B. L. , Mulligan B. W.
Published: August 2009

The application of X-ray spectrochemical analysis to various materials has undergone marked expansion in recent years. Special examples from the authors' experiences in the analysis of cements and dental materials are cited. Difficulties in presenting a representative sample to the primary X-ray beam are described, together with means for minimizing these difficulties. Interelement corrections for the X-ray analysis of cement are discussed. References are given to the work of numerous investigators in this field.
The Use of Neutron Diffraction in the Study of the Properties of Matter
Authors: Legrand E.
Published: August 2009

In recent years neutron diffraction became an important tool in the study of the properties of matter. In structure research it is used to complete the information of X-ray diffraction measurements. To illustrate this, some examples will be given of recent investigations on carbides, cyanides, and oxides of heavier elements, where the neutron measurements have allowed either to determine the positions of the light atoms or to correct or refine earlier X-ray measurements. Neutrons have also been used in the study of the physical structure of materials. In this connection some measurements on preferential orientation and grain size will be described. However, the study of magnetic structures is perhaps the most specific topic for neutron diffraction techniques. It is mainly in this field that measurements have been made at the Mol laboratory. Some experiments on perovskite-like compounds will be described.
Impact of Nuclear Technology on Highway Engineering
Authors: Blackwell P. L.
Published: August 2009

Modern automotive transportation has necessitated the handling, processing, and testing of natural materials for highway construction far more wisely than in any previous era. New materials developed in the general area of advanced technology, as well as those specifically for highway purposes, are being used for building and maintaining the highway structure. Nuclear technology is rapidly being applied to the material phase of highway engineering as a tool for measuring and testing materials in the construction and maintenance operations. The performance of nondestructive determination of material suitability and the speed with which measurements can be made by nuclear methods provide better processing and construction controls. The flow of materials can be measured and tested by extremely small quantities of radioactive material. Such tracer techniques assist not only in material production but also in the design of the highway structure itself. Nuclear energy also has some promise for changing the consistency of inferior soils to produce a suitable engineering material. The potential impact on highway engineering by nuclear power and heat, and as an explosive for earth and rock excavation, will affect highway location, design, and construction procedures. These and other developments of nuclear technology will advance engineering methods and may, in the not-too-distant future, bring about new principles and technology in highway engineering.
A Radiometric Method for Determination of Moisture in Brick Walls
Authors: Rossinski B. , Przedecki T. , Stachowicz Z.
Published: August 2009

The experimental work described in this paper was based on the Compton effect for the scattering of gamma radiation. For measurements one used a set of apparatus provided with a probe to measure density and a counter with a feeder from an accumulator. A 5 mc cesium isotop (Cs-137) was the source of radiation. The research comprised the calibration of probe, building of an experimental wall in a sheet iron, and systematic measurements during the humidification by electroosmosis. As a result of the experiments one obtained lists of relations between radiation intensity and time, moisture and time, and radiation intensity and moisture.
The Basis for Future Developments of Hydrocarbon Analysis, 1855–1965
Authors: Kurtz S. S.
Published: August 2009

The title of this talk “The Basis For Future Developments of Hydrocarbon Analysis”, is a large order. It ia true that future work is always based on what has gone before, on what is currently known. It is also true that ideas and techniques currently unrelated to the petroleum industry may suddenly emerge as of primary importance in hydrocarbon analysis, because of the development of some previously unheard of analytical technique. In this paper, I will try to cover the development of hydrocarbon analysis up to the present time, and to do just a little speculating about the future. No matter how well this is done, I am sure that a few years hence some new factors will become important in hydrocarbon analysis, which we cannot now foresee. Hydrocarbon analysis seems to be that sort of a subject. The course of events is far from predictable, but this does not mean that a good knowledge of the background does not have real value. We believe that it has. In approaching this large order of historical material, I believe that the best feel for the forward march of events in hydrocarbon analysis can be achieved by considering periods. This means considering the advances in the petroleum industry broadly, since the analytical needs and demands changed and multiplied as the industry developed. I am not aware of any historical treatment of this subject in the literature, and therefore have undertaken to write a text for publication which, if I read it today, would keep me talking for several hours. I am supposed to wind up this talk in about 25 to 30 minutes, therefore I can only give you today a small part of what I am preparing for publication. In selecting items to present from the wealth of material available, I have tried to pick out what will be interesting, even though historically other items may be more important. Today, I hope to give you some feeling for the broad picture of analytical progress in our field over the last 110 years. I regret that the limitation of time will not permit a more precise historical balance than is possible in such a brief presentation.
Current and Future Applications of Hydrocarbon Analysis in Quality Control
Authors: Dawson Lewis C.
Published: August 2009

Chemical analysis are often superior and more economical methods of evaluating hydrocarbon quality than simulated performance tests are. Modern instrumental techniques, such as gas chromatography, mass spectrometry, and nuclear magnetic resonance have facilitated analysis of complex hydrocarbon mixtures. Performance qualities can, theoretically, be calculated by integrating the contributions of the individual components. Empirical tests tend to correlate poorly with performance, and some of the older tests do not reproduce well. The author recommends that in the future alternate analytical methods be carefully considered before simulated performance tests are adopted as standards.
Analysis of Kerosine and Gas Oils
Authors: Ehrler A. J. , Farrell R. E. , Ingber N. M. , Nawrocka I. M.
Published: August 2009

The integrated methods approach to the analysis of the kerosine and gas oil fractions (boiling range 400 to 650 F, C11 to C20) of petroleum is described. The authors show that any well-staffed laboratory with the proper instrumentation can analyze these hydrocarbons to the point of identifying individual components. However, they also point out that there are still questions concerning the reproducibility of these methods. Before these methods can be used in commercial contractual agreements, they must be standardized and have their precision established.
Introduction to Session IV
Authors: Ball J. S.
Published: August 2009

Presenting a group of papers on non-hydrocarbons in a symposium on hydrocarbon analysis appears like a case of mistaken identity. However, the mistake that must be avoided today is the non-identification of impurities in hydrocarbons. The determination of extraneous materials in hydrocarbons or hydrocarbon mixtures is important whether the impurities are hydrocarbons or non-hydrocarbons. Thus, it is one thing to analyze a sample of toluene and say it is 99.8 per cent toluene but unless the 0.2 per cent of material is identified, it can cast doubt on the suitability of the product to be used for many purposes. The group of papers which we have this afternoon discuss some of the ways in which extraneous materials may be identified. Two general trends of petroleum analysis problems are considered. One is the increasing activity of the petroleum industry in manufacturing chemicals - petrochemicals, if you please. New standards of purity have been brought to the chemical market place by this activity, and the ingenuity of the petroleum chemist has contributed much. A second trend is the use of heavier crude oils where the non-hydrocarbon content becomes greater. For some of these oils the non-hydrocarbon material may become almost predominant. Similar conditions would result if shale oil becomes a charge stock for petroleum processes. The separation and identification of sulfur and nitrogen compounds is a difficult and painstaking task, especially during the methods development stage. The papers this afternoon will cover the present status of such research and consider possible modifications for the future.
Identification of Ultraviolet-Sensitive Impurities in Petroleum Naphthalene
Authors: King R. W. , Warren R. W.
Published: August 2009

Modern separation and characterization techniques were used as the principal tools in a research investigation designed to reveal the nature of the impurities that, if not carefully controlled, can cause color degradation of petroleum naphthalene. Substantially all of the hydrocarbon impurities present in a sample of petroleum naphthalene were identified. The presence of four indans, tetralin, five indenes and two dihydronaphthalenes was established. Accelerated ultraviolet exposure tests provided evidence that extremely pure naphthalene is quite color stable. Exposure tests on blends of pure naphthalene and hydrocarbons representative of those identified as impurities showed that methylindenes are uniquely deleterious to ultraviolet stability. Bromine index provides a measure of the concentration of these objectionable impurities that is adequate for quality control purposes.
Determination of Trace Hydrocarbon Impurities in High Purity Chemicals from Petroleum by Gas Chromatography
Authors: Klett R. A. , Korous L. R.
Published: August 2009

Gas chromatography, using packed columns and hydrogen flame-ionization detection, is used to identify and determine trace impurities in many high purity petrochemicals, such as benzene, cyclohexane, methyl cyclohexane, toluene, ethylbenzene, isopropylbenzene, styrene, -methylstyrene and propylene. Impurities in concentrations as low as 0.5 ppm may be detected. Using reproducible and equal volume injections, quantitative results are determined by comparing the detector response obtained for known levels of some impurity in a properly prepared standard blend with the detector response obtained for the impurities in a comparable sample.
Sulfur Compounds in Petroleum
Authors: Thompson C. J. , Coleman H. J. , Hopkins R. L. , Rall H. T.
Published: August 2009

The sulfur-containing constituents of petroleum have been of interest and concern to the petroleum industry almost since its beginning. However, only within the last 15 years has any significant progress been made in the identification of these sulfur compounds. This paper presents methods used in the isolation and identification of sulfur compounds and lists, by type or class, the 141 individual compounds identified in four crude oils by the Bureau of Mines-Am. Petroleum Inst. Research Project 48. Based on available techniques and identifications accomplished, suggestions are made relative to methods needed in future composition studies. The procedures described should have general application in the characterization of any crude oil.
Basic Nitrogen Compounds in Petroleum
Authors: Jewell D. M. , Yevich J. P. , Snyder R. E.
Published: August 2009

Methods used for the isolation and identification of basic nitrogen compounds in petroleum are reviewed. Analyses for these compounds in four types of oils: (1) jet fuel, (2) cracked and (3) hydrogenated light gas oils, and (4) heavy gas oils are compared to point out differences in the techniques used.
Nonbasic Nitrogen Compounds in Petroleum
Authors: Latham D. R. , Okuno I. , Haines W. E.
Published: August 2009

The status of knowledge about the nonbasic nitrogen compounds in petroleum is reviewed. Pyrroles, indoles, carbazoles, benzo-carbazoles, phenazines, benzonitriles, and amides have been identified in petroleum or its fractions boiling above 400 F. Nonbasic nitrogen can be divided into four subtypes by titration of the crude oil with perchloric acid in acetic anhydride before and after reduction with lithium aluminum hydride. This method requires no prior separation or concentration of the nitrogen, and provides more detailed information than previous methods. Future interest in nonbasic nitrogen lies in identification of classes of compounds in the heavier ends of crude oil.
Aspects of Linear Elution Adsorption Chromatography for Extraneous Materials
Authors: Snyder L. R.
Published: August 2009

the use of linear elution adsorption chromatography (LEAC) in petroleum separations is reviewed, as are previous applications of LEAC in the analysis of petroleum sulfur and nitrogen compound types. Future possibilities in the analysis for petroleum sulfur, nitrogen, and oxygen types by LEAC are discussed. The potential usefulness of such compound type determinations is briefly examined. Linear elution adsorption chromatography (LEAC) is a technique which appears quite promising for the rapid, routine analysis of petroleum samples according to compound type. The scope of this paper will be confined to applications of LEAC in the analysis of the so-called “extraneous materials” in petroleum: compounds containing sulfur, nitrogen, or oxygen. However, the technique is also useful in the analysis of the various hydrocarbon classes in petroleum (1–4). The discussion is in four parts: (l) some general observations on the LEAC technique per se, with particular reference to petroleum separations; (2) a review and evaluation of past applications of LEAC in the determination of various sulfur and nitrogen compound types; (3) a forecast of future possibilities of LEAC in the analysis of the extraneous materials in petroleum; and (4) a brief discussion of the potential usefulness of these analyses for the extraneous materials in petroleum.
General Factors in Design of Bituminous Paving Mixtures
Authors: Rader L. F.
Published: August 2009

The papers in this symposium present information on results of tests conducted primarily to determine stability. Other factors such as density, durability, and flexibility are also covered to some extent. The symposium papers pertain primarily to bituminous paving mixtures for highways and streets, but some phases are applicable to airport pavements. Before taking up the individual papers it is considered advisable to present a statement of general design factors that may serve as a framework for the concepts and data to be presented.
Theory and Application of a Gyratory Testing Machine for Hot-Mix Bituminous Pavement
Authors: McRae John L. , Foster Charles R.
Published: August 2009

In the design of dense-graded bituminous pavement, some means of establishing the maximum permissible bitumen content consistent with the anticipated type and intensity of traffic is required in the laboratory. Any amount of bitumen less than this is believed to be conducive to less than optimum durability, primarily because of reduced film thicknesses and a tendency toward greater porosity. It is desirable therefore to establish as narrow a limit below this maximum as practicable for field control. This upper limit appears to be best defined in terms of plasticity, that is, it is just below the bitumen content at which the pavement will shove or rut excessively under the imposed traffic. In order to predict this condition in the laboratory, it is necessary to produce a pavement sample having the anticipated prototype density. Also, it is desirable that the laboratory sample have stress-strain properties comparable to the prototype. A means of identifying the plastic condition directly rather than through the use of voids criteria, as now used, would be desirable. The gyratory kneading-type machine, originally conceived by personnel of the Texas State Highway Dept. for laboratory compaction, has been further developed to permit mechanical compaction of specimens to any given field condition. Indications are that it may be possible to evaluate the plastic properties of these specimens directly during the compaction process and thus indicate the optimum asphalt content. A procedure is proposed for designing and controlling the construction of pavement for heavy airplane traffic.
Application of the Marshall Method to Hot Mix Design
Authors: Lehmann H. L. , Adam Verdi
Published: August 2009

The primary purpose of this study was to determine the causes of extensive divergencies in test results obtained by different operators and different laboratories in the use of the Marshall test for hot mix design and to investigate discrepancies between laboratory-mixed and plant-mixed samples. The data and discussions presented are sufficient to draw some definite and some tentative conclusions. As to the reproducibility of test results, it can definitely be stated that: (1) the experience of the operator affects the results whenever hand mixing is used; (2) the mechanical mixer improves repeatabiliy but shows a tendency to give lower results for stability and specific gravity; (3) heating the breaking heads to 140 F improves test results; and (4) the viscosity of the asphalt at the time of mixing and compaction of the briquet affects the results. Pavement cores and molded specimens of plant mix show similar results. Rutting of a pavement seems to be affected by mixing procedure and by viscosity of bitumen at time of mixing and compaction. Specific gravities of samples mixed at plants are higher than those for mixtures prepared in the laboratory, which affects the apparent optimum asphalt content. Further tests are under way to establish the causes of this discrepancy. The laboratory density obtained by 50 blows of the hammer on each face of the specimen seems to correlate with field density obtained with pneumatic rollers. This study is not complete, and at the present time, definite conclusions should not be drawn. However it is unlikely that a change in the number of blows required for laboratory compaction in design studies will be necessary for present-day traffic. In conclusion, it can be stated that more research is needed to correlate laboratory mixing with pugmill mixing and that repeatability of results in using the Marshall method can be improved by taking several precautionary measures. Considering the conditions encountered in the field and the necessity of quick tests, the Marshall method is a valuable tool in hot mix design and control.
Correlation of Hveem Stabilometer and Cohesiometer Test Results and Kneading Compactor Densities with Service Records of Bituminous Pavements
Authors: Minor Carl E.
Published: August 2009

The state of Washington is divided by the Cascade Mountains into mild and moist coastal plains to the west and a much drier and seasonally hot and cold plateau to the east. Data based on experience in the state are presented to show that the design of a bituminous mix for maximum serviceability should be tempered to a considerable extent by its climatic environment and that the stabilometer, cohesiometer, and kneading compactor are useful tools in providing desirable design versatility. Densities obtained with the kneading compactor compare favorably with densities developed in the roadway after one or more years of service. Further data show that the density of a bituminous pavement generally decreases with depth and that the kneading compactor prepares a specimen with similar density distribution. Case histories of several selected bituminous pavements are presented and show that their service characteristics, particularly as related to plastic deformation, were forecast accurately by the stabilometer and cohesiometer. In conclusion, data are presented indicating that the following factors influence the serviceability of heavy-duty bituminous pavements: climatic environment of the pavement; quantity of asphalt; amount and type of dust; ratio of dust to sand; stabilometer and cohesiometer values of the mix; and weather conditions at time of placing. Where applicable, limiting numerical values for these various factors are suggested.
Introduction
Authors: Fink D. F.
Published: August 2009

This symposium was conceived two years ago as a result of a feeling by ASTM Committee D-4 on Road and Paving Materials that there was a need for a greater appreciation for and use of statistics by those responsible for the development and standardization of test methods for bituminous materials; and furthermore, that there was a real need for a better understanding of the practical significance of many of the test methods. I was particularly in sympathy with this attitude since I had recently attempted to secure acceptance of “statements of precision” for nine different tests on asphalt emulsions. I encountered considerable and, occasionally, heated divergence of opinion as to just how precision should be measured and expressed and even as to what practical significance could be attributed to any test result. Certainly no one can deny that, as a whole, tests on bituminous materials tend to be (a) largely empirical, (b) of dubious precision as far as engineering uses are concerned, and (c) only vaguely correlated with actual field performance of pavements. This is, of course, attributable to the historical background of paving technology. Most of the tests were designed originally to define the source rather than the nature of the material. With the years there has been an increasing tendency to transpose certain source-defining tests to performance-defining tests without any particular attempt at field correlation. Furthermore, levels of test precision which were entirely adequate for defining source may or may not be adequate when performance must be defined, as in writing so-called “quality” specifications. Even in the few cases in which test methods have been correlated with performance and engineering requirements, modern statistical concepts raise serious doubts about the validity of both the experiment design and interpretation of results. The testing of bituminous materials has not kept pace with testing of other materials of construction, for example, metals and plastics, both as to the level of precision attained and the degree to which properties of engineering significance are being measured. Continued full utilization of inexpensive and versatile bituminous materials in an atomic-age technology requires an up-to-date, precise description of their properties and capabilities.
Precision of Present ASTM Tests on Bitumens and Bituminous Materials
Authors: Brown A. B.
Published: August 2009

Those standards under the jurisdiction of ASTM Committee D-4 on Road and Paving Materials which deal with bitumens or bituminous compositions have been examined with respect to the adequacy of their precision claims. In many cases, precision statements are found to be inadequate in form, clarity, and coverage. Each method of test should include a precision statement which would specify (a) the range within which repeated determinations by the same operator on the same apparatus (repeatability) should agree; (b) the range within which check determinations by different operators on different sets of apparatus (reproducibility) should agree; and (c) the confidence level at which these ranges apply. It is recommended that Committee D-4 use a standard form of precision statement; that the inclusion of such be a requisite for every method of test; and that adequate supporting data be published or otherwise filed for ready availability.
Fundamental Statistical Concepts in Testing
Authors: Irick P. E.
Published: August 2009

Particular statistical techniques are discussed within a general description of statistical methodology. A simple comparative experiment is used to illustrate the general exposition. It is supposed that statistics aims to provide concepts, principles, and rules for obtaining consistency among three aspects of an experimental investigation: objectives, acquisition of data, and data analysis. The concepts of experimental universe and statistical model are taken to be fundamental to this purpose. An experimental universe is generated and sampled as a consequence of objectives and data acquisition designs. Objectives are reached by analyzing the data with respect to statistical models that represent associations among universe variables. Consistency of objectives, designs, and analysis for the example are attained by using the techniques of randomization, replication, estimation, and significance tests.
Density Changes in Asphalt Pavement Core Samples
Authors: Hein T. C. , Schmidt R. J.
Published: August 2009

A loss in density with time was observed on a large number of cores taken from experimental pavement sections made with a Corps of Engineers type asphaltic concrete. This change is rapid and can account for significant differences in results between laboratories. On other mixes, there is an increase in density. The change, therefore, is not predictable and is different with the different aggregates and mix designs used. Some of the change appears to be caused by a slow gain or loss in weight, presumably water. The rest of the change is caused by an increase or decrease in calculated volume of the specimen. This observation offers a basis on which to devise a more reliable procedure for determining the density of asphalt concrete pavements. It also questions the basis on which relative density requirements are set.