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By V. E. Homme

Low- and high-temperature reduction techniques were employed by the Bureau of Mines in study of conditions favorable to the formation of massive titanium crystals. '1,1,2 low-temperature method, feeding molten sodium to solidified titanium lower chloride-sodium chloride, produced higher quality and high quantity crystalline metal. The percentage of crystalline titanium was increased with increasing reactor diameter, melt depth, and titanium dichloride concentration. The high-temperature technique, feed molten sodium to melts above 8000 C, producing needle-type crystals of lower quality and with less consistent results than the low-temperature method. Layers of titanium foil, sponge, fine needles, wool, and crusts of sin-tered granules were formed during the earl, -art of the low-temperature reduction, and massive crystals were produced beneath this barrier in the latter part of the reduction. Crystalline titanium having an average hardness of Bhn 76 and representing 58 percent of the total titanium was obtained. Lamellar crystals up to 1 1/2 inches long with a hardness as low as Bhn 54 were also produced. A second-stage reduction for reclaiming titanium from offgrade sponge is described. Titanium produced by this method was comparable in quality to that from sodium reduction of titanium tetrachloride.

Jan 1, 1966

By John C. Machisak

Injury data and experience, with related employment statistics, at coal mines in the United States for 1960 are presented in this publication under the following general sections: A General injury experience: Tables 1 to 6: Current data on number of injuries, decree of injury, frequency and severity rates, average severity, and related employment and production data by work location. B Selected injury experience: Tables 7 to 38: Current data on principal agencies of injuries, distribution of injuries by part of body injured, days of disability, extent of hand and machine loading, experience by employment and production groups, and various other operating factors and physical conditions related to the occurrence of injuries at the Nation?s coal mines.

Jan 1, 1962

By Robert F. Chaiken

More than 500 fires are now burning in abandoned coal waste banks and coal deposits in the United States. Once established, such fires can burn for decades, and extinguishing them by conventional methods such as surface sealing to exclude air, excavation to remove fuel, or flushing to cool the fire zone is usually difficult and always expensive. Burnout Control, a technique developed by the Bureau of Mines for the control of abandoned coal fires, involves the accelerated combustion of coal in place with total management of the heat and fumes produced. A burning waste bank or mine is placed under negative pressure relative to the atmosphere, and heat and combustion products are drawn from the combustion zone through an exhaust ventilation system. Heat produced appears as sensible heat in the exhaust, at temperatures as high as 1,000° C (1,832° F), and could be recovered for the production of steam, hot water, process heat, or electricity. The Bureau's first field demonstration of Burnout Control was at Calamity Hollow in Allegheny County, PA (near Pittsburgh). Calamity Hollow was the site of an underground mine in the. 1900's and was surface mined in the 1940's. In the winter of 1961~62, a fire of undetermined origin was discovered in the exposed coal. In 1963, the Bureau constructed a trench barrier around the fire and a surface seal over the affected area. The fire was isolated but, not completely extinguished. In 1979, when the Bureau began work on the Calamity Hollow Mine Fire Project to demonstrate controlled burnout, the fire was still smoldering on the hot side of the trench barrier. The project, which was begun in December 1979 and ended in July 1982, consisted of the design, construction, operation, and subsequent dismantling of a Burnout Control ventilation system. This report, although considered part 2, is actually the last of a five-part series that describes the Calamity Hollow Mine Fire Project. It was written last because it involved the analysis of a substantial body of data describing in detail the results of a continuous 4-month burnout operation. The first report, part 1, describes the design and construction of the field installation. Part 3 describes the instrumentation used to control and monitor the progress of the burnout operation. Parts 4 and 5 deal with the closeout phase of the field demonstration. Part 4 describes the procedure used to quench the fire, and part 5 describes the final excavation and backfilling of the heated zones. The reports in this series document the Calamity Hollow controlled burnout demonstration, which showed that (1) controlled in situ combustion is a feasible method for controlling underground fires in abandoned mines, (2) the resultant thermal exhaust output is suffIcient for energy utilization, and (3) water injection-fume exhaustion is a potentially effective method for cooling large underground fire zones. Further investigations of both Burnout Control and the water injection-fume exhaustion quenching procedure are planned.

Jan 1, 1989

By John B. Gayle

A new, experimental coke oven was installed at the Southern Experiment Station, Tuscaloosa, Ala., in 1948. This oven, designated as the Tuscaloosa oven, features a 17-inch carbonizing chamber, globar heating elements, and silica-brick heating walls designed to simulate as closely as possible carbonizing conditions in commercial, slat-type coke ovens. Zoned heat-input arrangements maintain uniform temperatures over approximately 95 percent of the total flue area. The reasons for constructing an oven of this size, the details of the design, and the operating characteristics of the oven were given in an earlier publication.2/ This report presents the results obtained from the first series of carbonizing tests on Alabama coals with the new oven. Factors leading to the development of standardized operating and testing procedures and the results of crosscheck determinations with a commercial oven producing foundry coke are included also.

Jan 1, 1954

By Robert F. Chaiken

Burnout Control is a process developed by the U.S. Bureau of Mines for accelerating the burning of wasted coal fires in situ, while at the same time controlling the heat and fumes produced. The Albright fIre project is a fIrst fIeld trial of Burnout Control as applied to a coal waste bank. An exhaust ventilation system was designed and constructed and then operated over a 1-year period at the site of an existing abandoned mine land fire near the town of Albright, WV. While predicted exhaust gas temperatures of 900° C and thermal power levels of 5 MW were achieved at 20-to 3O-in H20 vacuum levels, problems were encountered with engineering designs, equipment breakdown, and fuel-rich combustion that curtailed the time period of satisfactory operation. Effective afterburning of the exhaust gases (as they were drawn from the bank) corrected the problems associated with combustion stoichiometry and led to high thermal outputs. It is believed that with (1) improvements in engineering design and construction, (2) better control of the afterburning process, and (3) the use of conventional stack gas air-pollution controls, Burnout Control can be applied successfully to a coal waste bank fire.

Jan 1, 1991

By O. P. Hood

The smoke problem means different things in different places . In the neighborhood of industrial plants , especially smelting plants and cement plants , the term " smoke " is applied to material discharged from these plants , consisting of a mixture of solid particles ( dust ) , fume which has condensed from vapors , and gases of various kinds that are produced in the operations . In the ordinary use of the word , however , " smoke" refers to the visible material which escapes from the burning of coal . White smoke usually owes its color to small drops of water which have condensed from the water vapor that it formed in the burning of coal . When smoke is black, the color is due to unconsumed particles of carbon and usually when the smoke problem is spoken of , it is this black smoke produced in the burning of coal that is referred to , Many inquiries in regard to smoke are addressed to the Bureau of Mines , and the following brief summary has been prepared as covering the usual questions . For references to the smoke problem in England , I am indebted to a recent interesting paper on this topic by David Brownlie .

Feb 1, 1922

By James H. Gary

Data regarding the composition and physical properties of Florida land-pebble phosphate-waste slime are presented, and the feasibility of dewatering and beneficiating the slime by several different methods is discussed. Chemical analyses, electron micrographs, and X-ray diffraction data showed that principal constituents of the slime included quartz, attapulgite, and flaorapatite. Viscosity of the slime changed with pH; thixotropic, Newtonian, and rheopectic states were observed as the pH increased. Use of various flocculating agents was not effective in improving thickening properties of the slime. Dewatering tests using pressure filtration showed that temperature influenced the filtration rate more than pressure; the filtration rate at 165° C was tenfold that at room temperature. Selective flotation of the slime, using two different processes, gave promising results. About 25 pct of the phosphate was recovered in a concentrate assaying 31 pct P205, Other tests demonstrated that the slime could be successfully fractionated at 20-microns using a hydrocyclone. In hydrometallurgical tests about 80 pct of the phosphorus and alumina were chemically extracted from the slime using sulfuric acid. Limited bacteriological studies made of the slime showed that several types of microorganisms were present and grew in the material despite the presence of fluorine-bearing minerals.

Jan 1, 1963

SMCRA contains five principal regulatory provisions that form the basis for its implementation: Performance Standards Performance standard safe intended to ensure that all surface mining is conducted in a way that protects the environment and the public and ensures that the mined land is restored to productive use following mining. Permits Before developing a surface or underground coal mine, an operator must have a permit issued under SMCRA. An application for a permit to conduct a surface coal mining operation is a detailed document that consists of text and numeric data describing the proposed mining and reclamation. Information must be furnished on pre-mining environmental conditions, existing land use, proposed mining and reclamation, how the performance standards will be met, and the post-mining land use. This provides the regulatory authority with the information necessary to determine that the operation can be conducted in accordance with the regulations. Performance Bonds Before a permit can be granted, an operator must post a performance bond sufficient to cover the cost of reclaiming the site in the event the operator fails to complete reclamation. The bond is not fully released until all performance standards have been met and reclamation of the site has been determined to be successful after five years in the East and Midwest, and after 10 years in the arid West. However, the bond can be partially released as various phases of reclamation are completed. Inspection and Enforcement If a violation of SMCRA or of a state surface mining and reclamation law is observed, an inspector issues a notice of violation to the operator. The violation must be corrected within a specific time, and the operator may also have to pay a fine based on the severity of the violation. If the violation is not corrected, acessation order is issued to immediately stop active coal mining, and the operator must pay a fine. If a violation is especially serious (for example, creates an Following reclamation, the land was immediately put back into agricultural production. Today, grain and corn crop yields have continually exceeded targets. 2 imminent danger to public health or safety or causes significant damage to land, air, or water resources) the inspector immediately issues a cessation order. An operator must correct all violations in order to obtain permits for new mines. Lands Unsuitable For Mining Congress recognized that certain coal deposits cannot be mined without permanent damage to unique cultural or natural resources. As a result, SMCRA protects these resources in two ways: It prohibits mining within the boundaries of national parks, forests, wildlife refuges, trails, wild and scenic rivers, wilderness and recreation areas; in areas which will adversely affect sites listed on the National Register of Historic Places; and within a restricted distance of occupied dwellings, public roads, buildings, parks, schools, churches, and cemeteries; and Provides a process that allows anyone whose interests may be adversely affected by proposed mining to petition to have specific lands designated unsuitable for mining.

Jan 1, 1992

By J. R. Thoenen

This paper outlines briefly results of seismic measurements recorded in the vicinity of quarry blasting under practical operating conditions. The data cover field work done from January to the middle of August 1930, during which time records were made of 61 blasts in 19 quarries. Of the tests made, one was in biotite-gneiss, two in dolomite, two in a flintlike volcanic complex, three in gabbrodiorite, five in trap rock, and six in limestone. One quarry was in Alabama, two were in South Carolina, two in New York, four in Kentucky, five in Connecticut, and five in Massachusetts. Explosive charges ranged from 0.30 pound to 41,900 pounds, and the method of shooting varied from mud caps through hammer and wagon drill holes to churn drill holes and coyote tunnel shots.

Jan 1, 1937

By C. R. Nisewanger, F. W. Brown

"The velocity of detonation of an explosive is one of its most important properties, because its performance depends markedly on the rate at which it releases its energy. Fortunately, the velocity of detonation is one of the few properties of an explosive that can be measured precisely. However, the velocity of detonation of an explosive may depend on several factors other than its chemical composition, such as density, physical state, degree of confinement, nature of confinement, and magnitude of initiating impulse. Presumably for an explosive of fixed chemical and physical properties there are certain limiting conditions of confinement and initiation under which the explosive will detonate at a maximum constant and uniform velocity. This velocity is its ""ideal"" velocity of detonation. It is obvious, however, that in order to evaluate performance properties of an explosive in all of its applications it may be necessary to measure its velocity of detonation under a number of conditions in which the velocity of detonation is far from the maximum ""ideal"" velocity.. Under certain-conditions the velocity of detonation may even,be,different at different points in the explosive.It is .relatively simple to determine the velocity of detonation of an explosive under a. standard set of conditions if one is free to use large quantities of the explosive and to form it into a convenient shape. Under these circumstances; one can use a thin column of explosive a meter or more in length. The time required for an explosion to travel the length of the column will not be less,of the order a few ten-thousandths of a second and can be readily and accurately measured .by means of the standard spark chronograph or by photographing the explosion with a rotating-drum camera. However in many applications the explosive charge may be of relatively small dimensions arid may not be in a form convenient for making velocity measurements and often may be enclosed in a case or other confining medium. It may be necessary to determine the velocity of detonation over distances of the order of a few centimeters, in which case the time intervals to be measured will be extremely small. For example, the time required for an explosion to traverse 1 centimeter of tetryl is of the order of 1.5 microseconds.Since no satisfactory method of determining time intervals of the order of magnitude of a few microseconds within an explosive charge was available,, at least not for all conditions that might be encountered in practice, it was necessary to develop a special electronic chronoscope which is capable of measuring time intervals as small as a microsecond with a fair degree of accuracy. This report describes the chronoscope and its application to measurements of velocities of detonation in explosives."

Mar 1, 1946

By R. L. Grayson

"Compliance standards for respirable dust, which are reduced because of high quart: concentrations, have become an industry-wide problem. Research on the physical and chemical character of quart-classified particles in respirable coal mine dusts indicates that they may exist in intermixed layers or may be coated by clay or coal material. The relative amount of intermixing varies with the coal seam being mined. If most of the quart: particles of a mine dust are ""pure,"" then the dust may have a high fibrogenic risk potential because of truly free silica and the compliance standard should be lowered. lf, however, quart: is locked inside another material matrix, or coated, a reduced compliance standard may not be appropriate.Although much research has been done on coal workers' pneumoconiosis (CWP) over the past decades, the etiologic agents of the disease still have not been pinpointed. The predominant methods of characterizing respirable coal mine dusts were bulk analysis techniques for determination of elemental and mineralogical concentrations, the results of which were used in statistical analyses to determine relationships between dust composition and the occurrence of CWP. These methods are incapable of finding the etiologic agents in the dust primarily because of complicated and confounding physiochemical factors, which may be discovered if the focus of characterization was done on a dust particle level.The SEM/EDXA-based research discussed here shows a significant difference in the number of ""pure"" quartz particles in respirable dusts collected from different mines. Some of the results have been reported previously (Grayson, Andre, and Simonyi, 1988). Concurrent research by other investigators (Wallace et al., 1989) demonstrates an SEM/EDXA-based methodology to pinpoint the location of the ""contaminating"" substance(s ) in a quartz-classified particle. The research of the European Economic Community has also begun analyses on the respirable-dust-particle level (Robock and Bauer, 1988).Since the compensatory and intangible costs of CWP are substantial in the United States, it is important that the etiologic agents be determined and then either controlled or neutralized in a cost-effective way. This line of research is especially important consid-ering the forecasted. near-term growth of coal production and the evolution of high productivity longwall panels (an immediate problem in compliance) and continuous mining sections ( a probable future problem).This need has been accentuated now that nearly all respirable dust samples submitted to MSHA are analyzed for free silica (Tomb, Parobeck, and Gem, 1986). Today a real problem exists in the coal industry, both underground and surface, because of high quartz levels in respirable dusts causing substantially reduced compliance standards (Murphy, 1989).The combined results of the respirable dust particle investigators indicate that conventional bulk sample analyses may not faithfully represent the amount of biologically available or active quartz in all mines with a high level (greater than 5% ) of quartz in the dust For example, some mine dusts might contain predominantly occluded (or coated) quartz particles where bulk analysis would result in anomalously high ""free silica"" measurements. The same result would occur when quartz particles are intermixed substantially with other minerals that can alter the surface of the composite particle away from a quartz-behaving character."

Mar 1, 1992

By Thomas M. Barczak

This Bureau of Mines report investigates shield mechanics by describing the elastic response and interaction of shield components to applied vertical and horizontal displacements for various canopy and base contact configurations. This research provides information on generalized shield mechanics, which is applicable in describing the behavior of all two-leg shield supports. Utilizing mechanics of materials concepts and known kinematic relationships for two-leg shield supports, free-body diagrams are constructed for each shield component illustrating internal axial, shear, and bending moment responses required to maintain equilibrium for each load case evaluated. Predicted shield (component) responses are verified by controlled displacement of instrumented longwall shields in the Bureau's mine roof simulator (MRS). Conclusions drawn from these analyses include shield structural responses are significantly dependent upon canopy and base contact configurations. Applied displacements also significantly affect shield responses. Horizontal displacement produces different responses than those produced by vertical displacements. The direction of horizontal displacement is also significant in evaluating shield response. Applications of shield mechanics to in situ support monitoring are also discussed. An objective of this research program is to establish unique shield responses to identify in situ load conditions.

Jan 1, 1989

Legislation and Government Programs.-On February 4, 1977, the Occupational Safety and Health Administration (OSHA) issued its final environmental impact statement on the occupational use of inorganic arsenic.2 The statement examined the ramifications of the original proposed standard published in the Draft Environmental Impact Statement (DEIS).3 The DEIS proposed to limit the exposure of employees to no more than 4 micrograms of arsenic per cubic meter of air as determined on an 8-hour-time-weighted average basis; or a ceiling limit of 10 micrograms of arsenic per cubic meter of air based on a 15 minute sampling period. The purpose of the proposed regulation is to reduce the risk of smelter workers developing lung and skin cancer as a result of exposure. A comprehensive study compiled by the Committee on Medical and Biologic Effects of Environmental Pollutants concluded that "there is strong epidemiologic evidence that inorganic arsenic is a skin and lung carcinogen in man."' In April 1977, the Environmental Protection Agency (EPA) served notice to ASARCO Incorporated that its Tacoma copper smelter and associated arsenic-producing facilities were in violation of State laws which limit sulfur dioxide and particulate matter emissions. This notice followed the Washington State Pollution Control Hearing Board overturning a prior ruling by the Puget Sound Air Pollution Control Agency (PSAPCA) which had permitted a 5-year variance from the State of Washington air quality standards. In December 1977, ASARCO appealed in court the decision of the Hearing Board.

Jan 1, 1980

By E. J. Murphy, A. P. Rowles, John C. Holtz

"INTRODUCTION The use of sheaths or hollow cylinders of flame-extinctive materials surrounding cartridges of permissible explosives has been developed during the last few years; the history of sheathed explosives in their salient development in Belgium was treated recently in a publication of the Bureau of Mines. 6/ This development is of great interest in explosives technology, for it holds possibilities of reducing further the ignition hazards that may cause many coal-mine disasters. The township interest in sheathed explosives in this country is attested by the passage of some State laws permitting the use of such explosives on shift 7/; inquiries are received in increasing numbers concerning the effects of sheaths on practical hazards as well as the general technology underlying their use."

May 1, 1943

By L. K. Weaver

The purposes of this Bureau of Mines report are to review the history of the domestic offshore hydrocarbon production; to project offshore oil and lease condensate production from 1971 through 1985; and to show the impact of offshore development on the onshore segment of the petroleum industry. Since 1954, offshore production has provided an increasingly larger portion of the domestic oil production. Domestic offshore oil and lease condensate production has increased from about 2.0 pct of the U.S. total in 1954 to 16.7 pct in 1970. Likewise, marketed gas production has increased from 1.0 pct of the U.S. total in 1954 to 15.0 pct in 1970. The past performance of exploration, leasing, development, and production of the offshore petroleum industry was used to make projections of offshore oil production. A comparison between onshore and offshore operations was also made. Assuming a tentative Department of the Interior offshore leasing schedule is completed by 1980, the authors estimate that by 1985, about 30 pct of domestic crude oil and lease condensate production from the lower 48 States will come from offshore areas. Currently, leasing of Federal offshore areas has been delayed due to environmental considerations. The rate at which off-shore hydrocarbons will enter the energy market will depend, to a large extent, on how soon environmental considerations are resolved. Assuming that offshore leasing will resume in the near future, U.S. offshore production of crude oil and lease condensate should be about 934 million barrels in 1985.

Jan 1, 1973

By R. R. Sayers

"An important, function of the U.S. Bureau of Mines is to instruct miners in first aid, and as a means of promoting interest in it first-aid contests are held under the auspices of the Bureau, usually in coop; ration with other interested organizations, especially the American Red Cross, the National Safety Council and various operators' and Miners' associations. It was early found that the method of judging first-aid meets is one of the most vital factors in determining the degree of success of the meet.It may be safely stated that there is no method for the judging of first-aid contests that has proved ideal. A method that would give the most uniform judging would necessitate the rating of each team by the same judge or committee of judges and, in order that a judge may rate a team satisfactorily, he should see that team perform several events and average the ratings. Such a procedure is not practicable where there are many terms entered in the contest, as it would prolong the meet indefinitely. To overcome this objection the method has been tried of assigning separate judges to each team but this brings in a new factor the individuality of the various judges, some of whom rate closely, others loosely. The next development was to average the judging by having the judges rate different teams for each event. This would seem to solve the problem out it has been found, after using the method over a wide area for a considerable period of time, that the differences in the judging are too marked to be at all satisfactory. The next development was to appoint a committee of chief judges three to five in number especially trained and experienced, to aid the individual judges in rating the teams. This method has proved satisfactory at small meets but, as committee must review the work of each judge on each event, it has not been deemed feasible for a large meet."

Nov 1, 1920

By R. Karl Zipf, Z. T. Bieniawski

"SummaryAs part of an effort.to understand the mechanics of fine fragment formation in coal, which is important in studies of respirable dust due to mining, fracture toughness measurements and the strain energy density (SEO) theory were applied to calculate the crush zone size under a cutting tool in coal. This · zone is the major source of fine fragments in the 1 to 10 µm size range. The model used in these calculations is a boundary element program containing a failure criterion based on the SEO theory. The boundary element program calculates linear elastic stresses at numerous points in the coal material ahead of a cutting bit. These stresses arc then input to a subroutine called critical ftaw length and orientation (CFLO) which uses the SED theory to determine the CFLO for a small crack at the boundary element stress computation point. The extent of crushing is based on earlier postulates about . the role of inherent flaws in a fragmentation process. To form 1 to 10 µm fragments requires firstly a local stress strong enough to activate flaws with a characteristic length less than 1 to 10 µm and secondly, a flaw density sufficient to provide an average spacing between flaws also on the order of 1 to 10 µm. The locus of active lO µm ftaws represents the maximum possible extent of fine fragmentation in the 10 µm or less size range assuming that a sufficient inherent flaw density exists. The approach offers a first order approximation to the extent of crushing under a tool tip. The size and shape of the crush zone volume is affected by the attack angle and geometry of the tool.IntroductionFine fragment generation in the 1 to 10 µm size range under the action of a generic coal cutting tool may be explained on the basis of fracture mechanics which suggests two major sources of fine fragments: first in a crush zone near the tool tip and second by shear fracturing. along major macrocrack surfaces (Zipf and Bieniawski, 1988a). In this paper, fracture toughness measurements and the strain energy density theory are used to calculate the crush zone size. This zone represents the major source of fine fragments in the 1 to 10 µm size range and understanding the mechanical factors controlling its size represents a first step toward using fracture mechanics to characterize the ·tendency of various coals to produce undesirable fine fragments."

Aug 31, 1989

By Harold M. Smith

Natural gas has been used as a fuel and source of energy almost from its discovery, but its use as a chemical raw material may be said to have begun in 1918, when Brooks and Humphrey3/ showed. presence of alcohols in the diluted acid oil obtained by the sulfuric acid-treatment of cracked petroleum distillates. However, development of the utilization of natural gas for chemical syntheses was slow, partly because erroneous ideas existed regarding the nonreactivity of tine hydrocarbons composing natural gas. Data accumulated by petroleum chemists throughout the world, particularly since about 1930, have shown that these hydrocarbons will react when activated by the effects of heat, pressure, chemical reagents, and light; also that the reactions can be made to proceed of practicable speeds and to provide good yields of useful products with moderate operating conditions, especially if catalysts are employed. As those results became known, the possibility of a synthetic organic chemical industry based upon these reactions became apparent, and today this industry is large and growing rapidly in importance. In this paper the story of the manufacture of chemical products from natural gas is told simply in graphic form. The industry is developing so rapidly that soma products may have been omitted, but every effort has been made to include all that are important or likely to become so. The difficulty of keeping information of this tape up to date is shown by reference to an information circular4/ or, the sore subject published by the Bureau of Mines in 1930, in which the important products are shown on a single chart, where as five charts are employed for the cane purpose at present.

Jan 1, 1940

By A. Z. Dimitroff

An improvised rock- dust disseminator, consisting of a 10-gallon galvanized metal milk can that dispenses rock dust in return air currents by the injection of compressed air has reduced the float dust explosion hazards at the Koehler coal mine, Koehler, N. Mex.

Jan 1, 1965

By C. H. Fisher, Abner Eisner

"INTRODUCTION Sulphuric acid of various concentrations has long been used as a reagent in the determination of olefins and aromatics in hydrocarbon oils 4 such as gasoline, kerosene, and neutral oils from coal—tar distillates. Despite its long use, however, there is no general agreement as to optimum conditions and concentration of acid, and numerous methods and modifications have been recommended. In most cases, treatment of the neutral oil with 60 to 90 percent sulphuric acid, followed by distillation to the original endpoint to remove olefin polymers, is recommended for the estimation of unsaturated hydrocarbons. The distillate thus obtained is taken as olefin—free oil and used in later stages of the anlysis. Aromatic hydrocarbons generally are determined in the olefin—free oil by suphonation with more concentrated acid (96 to 100 percent and fuming sulphuric acid are recommended), the hydrocarbons not attacked and removed as water—soluble sulphonic acids being considered as saturated hydrocarbons. In some cases the saturates are examined further by differentiatingbetween cyclic (naphthenes) and acyclic hydrocarbons (paraffins). Generally this is achieved by physical methods, although strong sulphuric acid is known to react preferentially with some types of saturated hydrocarbons,It was the purpose of the present work to make a general study of this type of analysis and to investigate the reactions of hydrocarbons under conditions often used in analyses that employ sulphuric acid reagents. Since previous work is not in good agreement, the optimum concentrations of acid for the different stages of the analysis were determined. Several sulphuric acid methods previously recommended and new modifications were compared, two synthetic solutions being used as the reference oil. The results obtained are presented below under separate headings."

Dec 1, 1937