bluuebunny/crossref_metadata_2025 huggingface dataset:
Application of Pyrolysis-Gas Chromatography to Qualitative and Quantitative Analysis of Polymers
Authors: Krishen A
Published: March 2009

Characterization of polymer mixtures presents a challenging problem and various techniques have been used for this purpose. One of the simpler methods is pyrolysis in an inert atmosphere followed by direct gas chromatographic analysis of the products. Precise control of the various experimental parameters makes it possible to obtain both qualitative and quantitative data on the polymeric constituents.

The gas chromatographic requirement for an instantaneous injection dictates that the size of the sample be small, the temperature rise should be fast, and the pyrolysis time be short. The Curie-point pyrolysis method comes close to meeting most of these requirements.

Characteristic gaseous products suitable for quantitation were obtained from polyisoprene, styrene-butadiene rubber, polybutadiene, ethylene-propylene-terpolymer rubber, and chlorobutyl rubber. The gas chromatographic conditions were designed to analyze the products which had a very wide range of volatilities. The flame ionization detection offered ample sensitivity for the detection of very small amounts of materials.

The use of absolute peak areas per unit weight of the sample resulted in simpler nonlogarithmic relationships which are suitable for automatic computer calculations.

Certain copolymers of unknown monomer ratio cannot be quantitated in the presence of other polymers containing the same monomeric unit. Monomer ratios in copolymers can be determined in other cases. When mixtures of known types of polymers are used their composition can be determined with a standard deviation of 1.5 percent.

This technique is recommended as a routine analytical method.
New Low Temperature Test Equipment for Rubbers
Authors: Eagles AE , Fletcher W
Published: March 2009

Poor reproducibility in the determination of low temperature properties of rubber has been investigated. The level of variability for three acrylonitrile rubber compounds in interlaboratory tests are quoted. The design of new equipment to overcome these difficulties using a simple dynamic test system is described. This incorporates a frictionless measurement system and allows for the determination of stress during a number of cycles of sinusoidal deformation at adjustable low frequencies. Tests are made on strips of rubber in tension and can allow for different levels of prestrain. To avoid errors due to bowing of the test strip a sliding lower grip is used. The effects of type of grip, intermittent and continuous oscillation, prestrain level, specimen size, test frequency, and rising or falling temperature have been investigated. Tests have covered a selection of different rubbers, and extensive evaluation of reproducibility has been carried out on nitrile rubbers of different plasticizer levels.
New Automatic Tensile Tester
Authors: Budd WJ
Published: March 2009

The traditional manual techniques required in preparation of samples and machine operation when performing stress-strain testing of elastomers have been a burden to laboratory managers for decades. When repeated in high volume, they became a significant cost factor. As a result, such testing became a prime area of study for automation.

To meet the demands for greater test production, higher reliability of information than was possible with the old methods, and to lower operating costs, Uniroyal developed the BUD II, a fully automated tensile tester. With this machine one operator, using only a minimum of time, prepares specimens and completes up to four times as many tests in a day as with earlier methods, while providing highly reliable and computerized information.
Tire Cord Fatigue Studies Using a Modified SCEF Tester
Authors: Lordi GJ , Prettyman IB , Forster MJ
Published: March 2009

Nine tire cord materials were evaluated on the Firestone SCEF fatigue tester modified to permit flexing at a series of angles (52.5 to 0 deg) including those used in bias and radial bodies, and in a cross-ply construction to simulate the cord interaction in bias body and belt constructions. Angle studies showed that whereas certain high modulus materials, such as fiberglass and Fiber B, would not be expected to flex well in bias bodies, they might in radial bodies. High angle flexing showed rayon poorer for fatigue than nylon or polyester, but equal in cross-ply. Other findings were the generally higher fatigue resistance (1) of the first than of the second generation Fiber B, and (2) of the higher than of the lower twists in each material comparison made. Fatigue results of belt candidates (rayon, fiberglass, Fiber B, polyvinyl alcohol, and nylon 66 obround monofil) differed widely, although all have shown durability in passenger tire belts. The preferred test angle for belt correlation has not yet been established.
Performance Evaluation of SO2 Monitoring Instruments
Authors: Purdue LJ
Published: March 2009

Continuous air monitoring sulfur dioxide (SO2) instruments which employ the four measuring principles most commonly used by federal, state, and local air pollution agencies are discussed. These measuring principles are colorimetry, conductivity, coulometry, and flame photometry. The advantages and disadvantages of using analyzers which employ each of these principles for collecting air quality data are discussed. Definitions for performance parameters and suggested performance specifications for SO2 analyzers are given.
Monitoring Oxides of Nitrogen — An Overview
Authors: Goldgraben GR
Published: March 2009

Oxides of nitrogen are an important parameter to be measured in ambient air monitoring, occupational health studies, source emission, and engine exhaust analyses. There are six commercially instrumented methods now available for their measurement: wet chemical colorimetric, chemiluminescence, electro-chemical, infrared, ultraviolet, and correlation spectrometry. These methods vary in sophistication, application, and cost and exhibit different advantages and disadvantages which must be considered in determining the most applicable instrument for a specific monitoring purpose.
Performance of Hydrocarbon Monitoring Instrumentation
Authors: Ortman GC , Thompson VL
Published: March 2009

Automatic instrumentation has evolved over the years to analyze the atmosphere for total hydrocarbon concentration, classes of hydrocarbons, and specific hydrocarbons. This paper deals with principles of analysis of commercial automated instruments—their performance, calibration, application, and impact on assisting our past, present, and future capability for measuring hydrocarbons.
Evaluation of New Ozone Monitoring Instruments by Measuring in Nonurban Atmospheres
Authors: Clark TA , Baumgardner RE , Stevens RK , Krost KJ
Published: March 2009

This paper compares the response and sampling characteristics of chemiluminescent ozone-ethylene monitors, the ultraviolet ozone photometer, and a solid phase chemiluminescent ozone monitor. Gas phase ozone-ethylene monitors from different manufacturers were used in the study to determine the differences in the response and sampling characteristics of some commercially representative monitors. Comparisons included correlation among instruments, typical response characteristics, and a detailed study of maintenance requirements and calibration stability.
Monitoring Trace Metal Particulates: An Evaluation of the Sampling and Analysis Problems
Authors: Skogerboe RK
Published: March 2009

A critique of current methods of monitoring trace metal particulates is presented in which sources of error in both the sample collection and analysis processes are pointed out. Results indicating that membrane-type filters are inefficient for collection of particulates in certain size ranges are presented and discussed. Possible problems with commonly used sample preparation and analysis procedures are pointed out and general recommendations for the elimination of these problems are made.
Recent Developments in IN SITU Size Spectrum Measurement of Submicron Aerosols
Authors: Husar RB
Published: March 2009

This paper reports the recent developments for in situ atmospheric aerosol size spectrometry in the diameter range below a few microns. Such particles are responsible for most of the visibility reduction and believed to be most dangerous to the human health. The use of optical single particle counters for aerosol size spectrometry is reviewed, and the main factors in counter design and aerosol characteristics affecting their performance are discussed. The paper reports the main characteristics of a modified Climet Instruments, Inc. counter, intended primarily for high size resolution atmospheric aerosol measurement in the 0.25 to 3.0 µm particle diameter range. Its main feature is an ellipsoid mirror scattered light collector. The design, operation, calibration, and size resolution of the University of Minnesota's Electrical Aerosol Analyzer is discussed. The instrument is capable of measuring aerosol size spectra in situ in the diameter range from about 0.004 to 0.5 µm with its size resolution being best at about 0.01 µm. A simple device, the diffusion battery can be used for rough size distribution measurement in the range 0.002 to 0.1 µm. Its principle of operation, design, and use is discussed.
Principles of Volumetric Analysis
Authors: Penkrot J
Published: March 2009

This paper presents the basic information concerning volumetric terms, types of volumetric glassware, and the calibration and the use of such glassware. Errors introduced by the use of this glassware are described. In addition, the different types of titrations are illustrated and discussed. The effect of dilution of the titrant on a typical acid-base titration using both indicator and potentiometric end points is discussed. Ethylenediamminetetraacetic acid titrations and their uses are also covered.
Dissolution of Metals for Analysis
Authors: Hobart EW , Kallmann S
Published: March 2009

The chemical analysis of any metal sample begins with dissolving of the sample. The intent of this paper is to demonstrate by means of a variety of examples the usefulness of a logical approach to metal dissolution considering oxidation and solvation as two distinct parts of the dissolution process.
Determination of Total Mercury Levels in Natural Waters
Authors: Nishi S , Horimoto Y
Published: March 2009

A rapid and simple preconcentration technique for the determination of trace amounts of mercury in natural waters has been studied. A 1-liter water sample is pretreated by conventional methods using permanganate and sulfuric acid. Mercury(II) ion formed is reduced to elemental mercury which is aerated and caught in a gold trap. The trapped mercury is released by heating the gold trap and driven into a photometer. A 0.01 ppb level of mercury in natural water is determined successfully.
Critical Review of Analytical Techniques for the Determination of Soluble Pollutant Heavy Metals in Seawater
Authors: Burrell DC , Lee M-L
Published: March 2009

The three most popular procedures for determining soluble trace heavy metal pollutants in seawater are: atomic absorption spectroscopy, thermal neutron activation analysis, and anodic stripping voltammetry. The applicability of these techniques are reviewed in terms of the respective detection limit capabilities, analytical difficulties imposed by the major ion matrix, chemical speciations, and pre-analysis preparation requirements.
Survey Analyses of Trace Elements in Water by Spark Source Mass Spectrometry
Authors: Crocker IH
Published: March 2009

The potential role of spark source mass spectrometry in water quality surveillance is perhaps not as widely appreciated as it should be. In this paper an attempt is made to explain what is unique about the technique and how it can augment other more widely used methods of analysis in the study of inorganic constituents of water.

At Chalk River it has been used to examine samples of water from several rivers, lakes, and streams. Most of the elements present in 100 ml of water in concentrations of at least one part in 1011 can be determined in a single analysis.

To date most other comprehensive evaluations of trace element concentrations in water have suffered from a lack either of sensitivity or of broad elemental coverage. It is probable that spark source mass spectrometry can remedy both of these shortcomings. Thus, it can fulfill a path-finding role in studies of toxic, dietary significant, or other especially interesting trace elements.
Rapid Determination of Cyanide in Waste Waters
Authors: Bhargava OP , Deline GW , Hines WG
Published: March 2009

A simple, direct, and rapid method is presented for the determination of cyanide in waste waters employing a selective ion electrode. The method can tolerate up to 100 ppm of sulfide in the sample and incidentally detects sulfide down to 0.05 ppm. The range of the method is 0.03 to 100 ppm cyanide and a single determination can be completed in about 3 min including the filtration of sulfide, if present, in the sample. The method has been in routine operation for about three years.
Guidelines for Quantitative Liquid-Liquid Extraction of Organophosphate Pesticides from Water
Authors: Suffet IH , Wu C , Wong DTL
Published: March 2009

A systematic approach for the development of quantitative analysis of organophosphate pesticides from water is presented. Information is presented on the different steps of aqueous pesticide residue analysis including liquid-liquid extraction, water and solvent phase separation, solvent drying, and a two-step evaporation of the extract which permits solvent volume reduction to 0.5 ml for recovery at low levels.

The p-value method of approach is used as a guide to optimize the liquid-liquid extraction step. The p-value determined in water is shown to be applicable to other types of water including river water, sea water, and secondary sewage effluent. Recovery studies are presented at nanogram/liter concentrations where the solvent evaporation procedure is shown to be critical.
Pesticide Residue Screening Methods Utilizing Multidetector Configurations
Authors: McLeod HA , Coffin DE
Published: March 2009

Multiple detection systems are reviewed as an approach to improve selectivity, increase the number of compounds detected, aid in confirming identity, and reduce the time of analysis. Various configurations of separators, detectors, and operating parameters are outlined. The advantages, disadvantages, scope, and practical application to screening biological samples for organic residues are illustrated by reference to several published methods for pesticide residues and drugs.
Uncoated Teflon as Support and Stationary Phase for Liquid/Solid Gas Chromatography
Authors: Kaiser KLE
Published: March 2009

The use of Teflon, 30–60 mesh, as a combined support and stationary phase for liquid/solid gas chromatography has been studied. The Teflon columns have separation properties similar to porous polymer supports. They exhibit short retention times at relatively low operating temperatures, durability, and low bleed. The chromatograms suggest that pure Teflon columns are suitable for the separation of hydrocarbons, alcohols, phenols, polychlorinated biphenyls, esters, and free fatty acids as well as for direct aqueous injections, such as the determination of methanol in water.
Gas Chromatographic Determination of Low Concentrations of Hydrocarbons in Water by Vapor Phase Extraction
Authors: Mackay D , Shiu WY , Wolkoff AW
Published: March 2009

A novel system for the measurement of low concentrations of hydrocarbons in water is described. The apparatus introduces a vapor sample of the hydrocarbon to a gas chromatograph following transfer of part of the hydrocarbon from the aqueous solution to a vapor phase. The thermodynamic basis for predicting the vapor-liquid equilibration is given. The method is capable of analyzing hydrocarbon concentrations in parts per billion range; however, the sensitivity depends on the hydrocarbon solubility and vapor pressure.
Experiences in Operating a Continuous Water Quality Monitoring Network
Authors: Hagan JE , Estes RL
Published: March 2009

Experiences in operating a network of continuous water quality monitors in the southeastern United States have demonstrated the utility of such networks for pollution abatement monitoring. Operation and maintenance procedures and routine calibration and quality control procedures produce highly reliable data. While local cooperators are necessary for economic reasons, the vital role of the trained electronic technician cannot be overemphasized.

Modifications and technical improvements to monitoring equipment are discussed. Problems encountered have been primarily mechanical in nature, particularly pumps.

Computer programs and semiautomated data handling systems have been developed to produce timely reports.
Sensors for Monitoring Water Quality
Authors: Ingols RS , Craft TF
Published: March 2009

Scientific principles of operation and general design considerations are given for sensors to monitor dissolved oxygen, turbidity, pH, conductivity, temperature, BOD. and specific ions. The importance of proper sampling procedures to the acquisition of valid data is emphasized. Solutions to problems encountered with continuous and semicontinuous monitors in the field and laboratory are detailed.
REX, A Computer Controlled Robot for In Situ Water Quality Monitoring
Authors: Birch KN
Published: March 2009

A new, computer oriented system for automatic in situ monitoring of water quality is proposed which makes full and effective use of modern computer technology. A concept for in situ computer controlled experimenting is developed as a reasonable and effective means of automatically observing the wide range of acquatic parameters needed.

The established capability in the teleprocessing industry is assumed as starting point and an optimal design is sought for a sensing head which would meet current expression of requirements for automated water quality monitors while exploiting the advantages of both hardware and software in a total system context. A working model of such a sensing head was constructed and operationally tested using an EAI 690 hybrid computer to simulate the central computer and telecommunications facility. This sensing head consisted of a peristaltic pump, a servo positioned valve, an array of six electrodes (2 glass pH, 3 silver-silver chloride, and 1 gold micro-electrode) and a thermistor, along with buffer amplifiers and motor controllers to service these devices. A main feature is its design as a remote, computer periferal, like a teletype, which understands up to 64 different commands and which returns coded responses. A second feature is its in situ design making the entire sensor head submersible and operable in depths to 100 m.

A repertoire of programmed experiments was developed for the working model system to show how, for example, it could monitor the water quality parameters; temperature, pH, conductivity, dissolved oxygen, chloride ion, total carbon dioxide, total alkalinity, and a factor called “other ions.”
Environmental Impact of Experimental Oil Spills in the Canadian Arctic
Authors: Adams WA , Scott BF , Snow NB
Published: March 2009

In August 1973, oil spills (using two different crude oils) were carried out near Inuvik, in the Mackenzie River Delta. One oil was from the Canadian Subarctic at Norman Wells, and the other was from the Pembina oil field in Alberta. Each oil was poured into a separate typical productive Delta lake that had been partitioned to provide a spill and a control area. Bioassays of water and sediment were regularly determined, as was the dissolved oxygen content, for each spill. Samples were taken of the weathered bulk oil. For the spill involving Norman Wells crude, incident solar radiation and temperature were continuously monitored at various depths below the oil and compared to the control area. Results obtained during the first two weeks of the spill will be discussed.
Sampling Techniques in Urban Runoff Quality Studies
Authors: Marsalek J
Published: March 2009

Composite as well as sequential sampling techniques are examined with regard to their applicability in urban runoff studies. While inexpensive composite sampling is adequate for the determination of the total pollutant yield from a watershed, the study of variation in pollutant concentration requires sequential sampling.

A rational approach to the development of a sequential sampling program is proposed, weighing the cost of data acquisition against the detail and significance of the information obtained. The design of such a program is based on the adoption of an empirical model for the variation of runoff quality and on the techniques of prediction analysis.

Practical aspects of sampling installations are also considered. Such considerations include the depth of sample withdrawal in a nonhomogeneous media, the capability of a sampler to collect solids, sample cross-contamination, and synchronization between flow records and collected samples.
Stable Carbon Isotope Ratios as Water Quality Indicators
Authors: Tan FC , Pearson GJ
Published: March 2009

Stable carbon isotope ratios (C13/C12) of man-made organic substances such as petrochemicals and pulp mill effluents are generally different from those of the “natural” organic matter in marine environments. By measuring the C13/C12 ratios of background organic matter in the marine environment and the pollution sources, an estimate of the degree of man-made pollution can be obtained.

Principles of the CO13/C12 technique, analytical methods, and an example of its use are discussed together with the limits of applicability of the approach.
Data Are for Looking At or Quality Control Through Interpretation
Authors: Bewers JM , Macaulay ID , Sundby B , Buckley DE
Published: March 2009

A logical interpretive procedure for the examination of environmental data is described and its use illustrated. The procedure is used to eliminate errors, detect redundancies, detect and validate anomalies, examine water quality data sets, and improve analytical and sampling techniques. It is a first step towards thorough data analysis and should ensure that the data, which are subsequently used for geochemical or environmental purposes, are valid.
Study of the Sand Patch and Outflow Meter Methods of Pavement Surface Texture Measurement
Authors: Doty RN
Published: March 2009

A study of the sand-patch and outflow meter methods of pavement surface texture measurement was completed. Included in this study were repeatability testing and testing to determine the degree to which pavement surface texture, as measured by these procedures, correlates with pavement coefficient of friction, skid number, and skid number speed gradient. Test locations were selected on open-graded and dense-graded asphalt concrete, chip-sealed and fog-sealed asphalt concrete, and new, polished, and grooved portland cement concrete (PCC) pavements. The results of the testing indicated that the repeatability of the sand patch test procedures studied was poor to fair and that the outflow meter test results were independent of water temperature. A general trend toward higher skid numbers and coefficients of friction was evident with increasing texture depth, as measured with both the modified sand patch and the outflow meter procedures. However, neither relationship was considered definitive enough to use as a basis for a minimum texture depth construction specification requirement for pavement surfaces. Also, neither method provided a definitive measure of skid number speed gradient.
Design of Texture in Standard Surfaces
Authors: Moore DF
Published: March 2009

All engineering surfaces exhibit varying degrees of sharpness and roundedness, and this characteristic is commonly identified by the “feel” or touch of the surface under consideration. Model surfaces such as cubes, cones, and spheres demonstrate extremes of flatness, sharpness, and roundedness, respectively, and they have the dual advantage of simple mathematical definition and reproducibility. This paper describes a logical progression from model to random textures, and discusses the relative significance of mean void width and asperity size, shape, and spacing. An alternating mechanism of wear on road surfaces is shown to exist which preserves the macrotexture by successive flattening and rounding of individual asperities. It is concluded that the two fundamental requirements of any standard surface are minimal wear and reproducibility or repeatability of frictional results. These criteria demand some degree of compromise in establishing a desirable texture in a standard surface, whereas the resulting frictional performance of the final selection is of secondary importance.
Interactive Tire Designs
Authors: Clark SK
Published: March 2009

The principle of utilizing geometric interaction between runway asperities and tire pattern design is discussed, and a theoretical basis is presented for substantial enhancement of frictional effects by this process. Test data confirming this is given. First order analytical expressions are given for the increased friction coefficients and for the engagement distances required. High-speed friction data on a 7.00 × 8 aircraft tire is presented confirming this. Example design geometries are shown for the tire tread groove pattern, and designs and materials are discussed for the asperity grid and its attachment system.
Pavement Surface Information Needs in Accident Investigation
Authors: Hutchinson JW , Tsongos NG , Bennett RC , Fogarty WJ
Published: March 2009

This paper summarizes some needed information on pavement surface characteristics for in-depth multidisciplinary traffic accident investigation, with emphasis on the variations and confounding effects of factors which are either not sufficiently researched or not properly appreciated and controlled in accident investigation.
Texture, Skid Resistance, and the Stability of Automobiles in Limit Maneuvers
Authors: Hayes GG , Ivey DL
Published: March 2009

The capability of conventional automobile/tire systems to perform a variety of emergency maneuvers was determined. In general, this capability was quantified in terms of the maximum values of longitudinal and transverse vehicle accelerations that could be produced under specific conditions. These vehicle/tire performance measurements are compared directly with common indicators of available friction such as texture measurements and skid numbers. The texture measurements appear to correlate as well with vehicle performance as do direct friction measurements such as skid numbers and British Pendulum Numbers.
Some Quantitative Aspects of the X-Ray Photoelectron Spectroscopy Analysis of Metal and Oxide Surfaces
Authors: McIntyre NS , Cook MG
Published: March 2009

Using metal and metal oxide surfaces as examples, three aspects of quantitative X-ray photoelectron spectoscopy are discussed, namely, the effects of surface contamination and structure, dilution effects in mixtures, and the influences of stoichiometry on photoelectron intensity ratios. The intensity attenuating effect of carbon was determined for several types of surfaces, and, in all cases, a quasi-linear relationship was found between the intensities of carbon and those of the specimen matrix. The slope of the line is dependent upon the surface structure of the matrix as well as well as the kinetic energy of the matrix photoelectron. Excess oxygen in an oxide matrix has little effect on the metal and oxide line intensities, but heavy metal impurities incorporated into the surface strongly attenuate the matrix lines. The metal line intensities from copper-nickel and iron-nickel alloys were determined as a function of composition. The intensity of each component varied linearly with the atomic fraction indicating that the electron scattering cross section is not significantly different in these metals or their alloys. Quantitative measurement of these surfaces is practical only when the more deeply probing M(3p) electon lines are used. Oxygen/metal photoelectron intensity ratios are a reproducible property of a particular oxide. Their ratios, however, are altered not only by changes in stoichiometry, but to some extent by changes in structure. Quantitative analysis of an oxide surface is thus reliable only for specimens where the oxide structure is identical to the standard throughout the compositional range of interest.
ESCA Studies of Nickel-Boron Electroless Coatings
Authors: Swingle RS , Ginnard CR , Madden GI
Published: March 2009

Electron spectroscopy for chemical analysis (ESCA) has been used to study the surface chemistry of electroless nickel-boron coatings. Changes in relative surface composition and element oxidation state were observed for boron, nickel, thallium, and sulfur as the coating was heated at 10-5 torr and heated in air. Under these conditions, boron was more easily oxidized than nickel, accounting for the oxidation resistance of the coating as compared to nickel metal. A small portion of sulfate stabilizer in the coating bath was reduced to sulfide and codeposited during the electroless plating process.
Composition of Protective Films Formed on Iron and Stainless Steels
Authors: Lumsden JB , Staehle RW
Published: March 2009

The composition of passive films formed on austenitic stainless steels have been determined using Auger electron spectroscopy. The films were found to be enriched in chromium which is consistent with the understanding of the relative insolubility of chromium compared to that of iron and nickel. However, the films were depleted in both silicon and molybdenum which are thermodynamically more stable than chromium in the solutions used. Thus, it is not possible to rationalize the improved resistance to acid solutions and solutions containing chlorides obtained by the addition of silicon and molybdenum to stainless steels using a selective-dissolution-enrichment model.
Determination of the Low Temperature Diffusion of Chromium Through Gold Films by Ion Scattering Spectroscopy and Auger Electron Spectroscopy
Authors: Nelson GC , Holloway PH
Published: March 2009

The transport of chromium through thin gold films has been characterized by ion scattering spectroscopy and Auger electron spectroscopy. The dominant transport path was shown to be grain boundaries in the gold films. The driving forces for transport were shown to be the reduction in the systems free energy associated both with the free energy of mixing and the free energy of formation of chromium oxide (Cr2O3). The kinetics of grain boundary diffusion were determined as a function of time and temperature. The grain boundary diffusion coefficient preexponential was determined to be 3.8 × 10-3 cm2/s and the activation energy to be 26 kcal/mol.
Comparison of Evaporated Surface Coatings Using the Ion Scattering Spectrometer and the Auger Electron Spectrometer
Authors: Bingle WD
Published: March 2009

Ion scattering and Auger spectrometry have proven to be useful analytical techniques for elemental analysis of surface composition. However, few, if any, previous studies have been made to show the variations that exist between the two analytical techniques. To better illustrate the difference in results between the two analytical techniques, a series of thin film evaporated coatings were prepared on different substrates for examination and analysis on both the ion scattering spectrometer (ISS) and Auger electron spectrometer (AES). Some basic agreement between the two techniques is noted; however, the variation with substrate and extraneous element concentrations shows that the characterization of material surfaces using ISS and AES demands further investigation and development before quantitative analyses can be attempted.
Small Area Depth Profiling with the Ion Microprobe
Authors: Whatley TA , Comaford DJ , Colby J , Miller P
Published: March 2009

The general technique of secondary ion mass spectrometry is now practiced in a number of instrumental variations. For certain problems, any one of these could usefully be employed. However, there is an important class of analytical problems that can be studied only with those instruments of the “small beam type,” that is, an ion microprobe. These problems are those of characterizing fabricated devices, principally in the solid state electronics industry. Regions to be studied on these devices are frequently only a few tens of microns in lateral dimension.

The technique has been applied, for example, to the study of adjacent base and emitter regions of a single transistor. Detailed concentration distributions, showing the influence of phosphorus on diffusion of boron double implants were obtained from 25 × 30-µm active areas of 100 × 150-µm rastered regions. Even smaller areas can be successfully analyzed by utilizing reduced beam diameters and a correspondingly reduced raster size. With presently available instrumentation, the practical lower limit on analyzed area is about 4 × 5µm (using a 2/to 3-µm beam and a raster size of 12 × 15 µm). At this level, problems of beam diameter, sensitivity, and surface contamination all become limiting.
Analysis of Solids Using a Quadrupole Mass Filter
Authors: Fralick RD , Roden HJ , Hinthorne JR
Published: March 2009

The quadrupole mass analyzer for solids (QMAS) is ideally suited for multielement analysis because of the rapid scanning capabilities of its quadrupole mass filter, the high sensitivity inherent in the secondary ion mass spectroscopy (SIMS) technique, and an instrumental configuration which produces abundance sensitivities in excess of 105 to 1. These capabilities allow the elemental composition of solid specimens to be readily measured and permit the detection of contaminants and dopants on the surface as well as in the bulk of a specimen to be determined. A typical mass survey of a silicon specimen is shown and some of its features are discussed. Because of the correlation between the time of sputtering and the depth eroded into a specimen, multiple element in-depth profiles are also readily measured with QMAS. In-depth distributions of boron and phosphorus, both implanted and diffused into silicon, have been determined and are discussed. The effects of different specimen treatment histories are found to be reflected in the depth profiles obtained.

In addition to depth profiling, the instrument has been used successfully for isotope ratioing. Work done with the lead isotopes indicates that the accuracy of the measured ratios is limited only by counting statistics. The accuracy of these analyses verifies that the instrument can be used routinely to analyze insulators. These studies also illustrate that spectral ion interferences can often be successfully treated by peak stripping techniques. In the same study, the analytical problems associated with possible mass discrimination and the ability to obtain quantitative elemental analyses have been investigated and the results compared with the ion microprobe mass analyzer (IMMA).
Effect of Water Saturation History on the Strength of Low-Porosity Rocks
Authors: Ballivy G , Ladanyi B , Gill DE
Published: March 2009

The purpose of the tests described in this paper was to investigate how the mechanical properties of rock observed in the tests are influenced by the whole saturation history of the specimen prior to testing. Three aspects of the saturation history were studied in this paper: the effect of drying and resaturating the specimen prior to testing, the effect of resaturation method, and the effect of the chemical nature of the resaturating fluid. Three rock types were used in the tests: a gneiss, a cemented sandstone, and a fine grained limestone. All three rocks had apparent porosities below 2 percent.

Results of triaxial and splitting tests are reported in the paper. One series of specimens was brought from the site in its natural saturated state and tested without drying while the others were either air or oven dried and then resaturated prior to testing. The resaturation was performed either by immersing the specimen in water under vacuum, or by injecting the saturation fluid, under pressure, through a thin channel drilled along the specimen axis. Either distilled or seawater were used as the resaturating fluid.

The results show that the inclusion of a drying and wetting cycle prior to testing has a clear overconsolidation effect on the rock behavior, that is, it increases its apparent strength. On the other hand, the channel saturation technique gives a better saturation of the specimen and results in a strength decrease. Finally, the results show that the chemical composition of the saturation fluid has also a significant effect on the measured rock strength.

The practical conclusion to be drawn from this study is that representative rock samples, taken in connection with a given project, should, from the moment of coring until they are tested, be held under environmental conditions that are as close as possible to those which will prevail after the completion of the project. This implies that no drying and wetting cycles should be included if they are not expected to occur in practice. If this condition cannot be met, specimens should be saturated using a natural saturation fluid and using an efficient saturation technique such as the described axial channel saturation method.
Trimming Device for Obtaining Direct Shear Specimens from Samples of Stiff Fissured Clay Shale
Authors: Durham GN
Published: March 2009

A device has been developed at the U. S. Army Engineer Waterways Experiment Station for obtaining direct shear specimens of hard, brittle soils, the use of which has resulted in a reduction in man-hours for specimen preparation from 3 or 4 h to 50 or 60 min per specimen. This device, which has proved to be superior to any previous apparatus used for obtaining direct shear specimens of such soils, is fitted to the base of a commercially available unconfined compression apparatus of the hand-operated type. Samples found untrimmable heretofore can now be tested, because a sample is held rigidly during trimming operations, and the time of exposure to air drying (and subsequent deterioration) has been reduced substantially.
Effects of Storage and Extrusion on Sample Properties
Authors: Arman A , McManis KL
Published: March 2009

The shear strength of specimens obtained with thin-walled tubes decreased as a result of long-term storage. The preconsolidation pressure of stored tube samples also followed a similar trend. Specimens obtained from hand-cut blocks did not show a decrease in strength or preconsolidation pressure with time. Samples stored by wrapping in plastic film and aluminum foil were found to be preserved as well as those stored after coating with paraffin. Stresses applied to samples for extruding from thin-walled tubes were found to be in excess of the shear strength of the soils. X-ray radiographs of specimens obtained with thin-walled tubes showed excessive disturbances caused by sampling and extrusion.
Compaction and Preparation of Soil Specimens for Oedometer Testing
Authors: Booth AR
Published: March 2009

The paper describes the development of a method for the compaction of groups of identical oedometer specimens. Groups were compacted from several soils at various densities and moisture contents. The specimens in each group were tested later in the oedometer over the complete range of initial saturations, and it was important that they should be as near as possible to identical after compaction.

The paper considers, by means of a literature review, the various methods of compaction available. The conclusion reached is that the static method is most suitable for compaction of relatively thin specimens. Soil was compacted directly into the oedometer rings under static loading. The advantages and disadvantages of this approach are discussed.

A special mold developed for this purpose is described in detail. This enabled a known mass of soil to be compacted into a 76.2 by 19.05-mm-thick specimen. The procedure used in the laboratory is outlined.

It was necessary to allow most specimens to either increase or decrease in moisture content after compaction so that oedometer tests could be carried out over the complete range of saturation. The procedures followed are described, and it is stressed that these model as closely as possible what would happen in a road embankment.

Finally, the paper considers the dry densities of groups of specimens immediately prior to being placed in the oedometer. It is shown that variations within each group are lower than those found in undisturbed samples, and it is concluded that the standardized method produced groups of specimens which were closer to identical than would have been obtained by other methods. This, in turn, enabled the influence of other variables, principally the compaction moisture content and initial dry density, to be studied with more confidence.
Laboratory Preparation of Specimens for Simulating Field Moisture Conditions of Partially Saturated Soils
Authors: Chu TY , Chen SN
Published: March 2009

Due to the significant effect of soil moisture on the behavior characteristics of a soil, one of the primary requirements in the preparation of specimens of a partially saturated soil is to simulate the suction in the soil under prevalent field conditons. This objective may be achieved by the conditioning or pretesting treatment of a soil specimen, so that a desired suction in the specimen is attained prior to testing. Relatively simple equipment such as that described in this paper, is suitable for the required treatment of specimens representing partially saturated soils. This paper presents results of undrained triaxial tests and repeated loading tests on soil specimens treated by using the equipment mentioned previously. Test data from specimens without any suction treatment are presented for comparison purposes. Information obtained from these experiments indicates that the simulation of the field moisture condition of a soil cannot be achieved simply by reproducing the field moisture content of the soil. The conditioning or pretesting treatment of soil specimens by using apparatus such as that presented in this paper is believed to be a preferable method for the purpose of simulating field moisture conditions.
Study of Irregular Compaction Curves
Authors: Lee PY
Published: March 2009

Curves of dry density versus moisture content, as yielded by the standard ASTM compaction tests, usually show a single maximum, but some soils exhibit compaction curves with irregular shapes. This study examines some of the influences of soil preparation on these irregular compaction curves. When a surface tension reducing agent, such as aerosol-AY, is added to the water in soil specimen preparation, the shape of the irregular compaction curve will be altered. This effect is regarded as a verification of the effects of negative pore water pressure on the irregular compaction curve. In repeated compaction tests, it is economical and convenient to reuse the soil specimens. The results of liquid and plastic limit tests reveal approximately the same values in new and reused specimens. However, the reused soil specimens reveal a predominantly higher density in the zone of lower water content in an irregular compaction curve.
Soil Drying by Microwave Oven
Authors: Lade PV , Nejadi-Babadai H
Published: March 2009

An investigation of the usefulness of the microwave oven for water content determination and for drying of soil before testing was performed. Soils ranging from highly plastic clays to clean sand were used. The influences of initial water content, amount of soil, and soil type on the drying time were investigated. Differences between water content determined using a microwave oven and a conventional oven decreased with decreasing plasticity of the soils. The microwave oven can be used for quick drying of soil, but accurate determinations of water content may only be achieved for nonplastic soils such as coarse silts, sands, and gravels. The change in classification according to the Atterberg limits was taken as a measure of the effects of heating by microwaves. The plasticity and swelling potential of the soils decreased after preheating in the microwave oven, and these effects are comparable to the effects of drying the soils in a conventional oven at high temperatures.
The Influence of State of Stress on Low-Cycle Fatigue of Structural Materials: A Literature Survey and Interpretive Report
Authors: Krempl E
Published: March 2009

Description

A comprehensive literature survey and interpretive report of interest to metallurgists and design engineers.
Field Testing and Instrumentation of Rock
Authors: Clark GB
Published: March 2009

Description

The symposium on Field Testing and Instrumentation of Rock was given at the Seventy-sixth Annual Meeting of the American Society for Testing and Materials held in Philadelphia, Pa., 24—29 June 1973. Committee D18 on Soil and Rock for Engineering Purposes sponsored the symposium. G. B. Clark, University of Missouri-Rolla, presided as symposium chairman.
Determination of The Spectrochemical Working Curve
Authors: Mason GL
Published: March 2009

Description

Two audio tapes present 3 hours of lectures comprised of five papers. Accompanied by illustrated booklet.
Handbook Of Fatigue Testing
Authors: Swanson SR
Published: March 2009

Description

In 1949 Committee E-9 on Fatigue published ASTM STP 91, Manual of Fatigue Testing. The project leading to STP 91 involved the specific writing of eight members of E09 and the discussions and criticisms of members of the main committee over a period of three years. STP 91 was a modest effort and succeeded in presenting what was then considered to be the current practice and views of E09 members.
Bearing Steels: The Rating of Nonmetallic Inclusion
Authors: Hoo JJC , Kilhefner PT , Donze JJ
Published: March 2009

Description

The symposium on Rating of Nonmetallic Inclusion in Bearing Steels was presented at May Committee Week of the American Society for Testing and Materials held in Boston, Mass., 22-24 May 1974. Committee A01 on Steel, Stainless Steel, and Related Alloys, Subcommittee A01.28 on Bearing Steels, sponsored the symposium. J. J. C. Hoo, FAG Bearing Corporation, presided as symposium chairman, and P. T. Kilhefner, Jr., U.S. Steel Corporation, and J. J. Donze, Timken Company, served as symposium co-chairmen.
Composite Reliability
Authors: Wu EM
Published: March 2009

Description

The symposium on Composite Reliability was presented in Las Vegas, Nev., 15-16 April 1974. The symposium was sponsored by Committee D30 on High Modulus Fibers and Their Composites, American Society for Testing and Materials, in cooperation with the American Institute of Aeronautics and Astronautics, American Society of Mechanical Engineers, and the American Institute of Mining, Metallurgical, and Petroleum Engineers. E. M. Wu, Washington University, presided as symposium chairman.
Practical Applications of Neutron Radiography and Gaging
Authors: Berger H
Published: March 2009

Description

The Symposium on Practical Applications of Neutron Radiography and Gaging was held at the National Bureau of Standards (NBS) in Gaithersburg, Md., on 10-11 Feb. 1975. The meeting was sponsored jointly by NBS and The American Society for Testing and Materials (ASTM). ASTM Committee E07 on Nondestructive Testing and Subcommittee E07.05 on Neutron Radiography were the ASTM sponsors. Several other organizations assisted in arrangements for the symposium. These cooperating societies include the Air Transport Association of America, the American Nuclear Society, the American Society for Nondestructive Testing, and the Nuclear Division of the American Society for Quality Control. Harold Berger, NBS, served as chairman of the symposium, and John K. Aman, E. I. du Pont de Nemours & Company, and Daniel Polansky, Naval Surface Weapons Center, served as cochairmen.