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Improve safety at mineral operations that use cyanide leach solutions to recover precious metals from finely ground ores, Approach Provide an alternative, non-acidic means of cleaning processing systems such as the State-of-Maine filter system, thereby reducing the exposure of workers to toxic hydrogen cyanide gas (HCN), The Problem Many gold and silver mining operations use cyanide solutions to dissolve gold and silver from ores. The precious metals frequently are recovered from pregnant leach solutions by the Merrill-Crowe recovery process, whereby gold and silver is precipitated with zinc dust. When that method is used, suspended particles in the leach solution must be filtered out before zinc precipitation can occur. This filtering is accomplished with small packaged plants, such as the State-of-Maine (SOM) filtering system. Unfortunately, the filters become clogged with calcium carbonate scale after about 2 to 10 days of operation and must be cleaned before further precious metals recovery operations can continue, Cleaning the system is a hazardous task because the acid is not compatible with the alkaline cyanide leach solutions, and toxic hydrogen cyanide (HCN) gas may be produced when the acid and solution are mixed. That gas, if breathed or contacted with the skin, can cause cyanosis which may induce nausea and even asphyxia and death. To reduce this danger, the Bureau of Mines has devised a safer method of cleaning clogged filters,

Jan 1, 1986

By Karl R. Becker

Detonators representing a sampling of various domestic commercial delay detonators were fired at various direct-current (dc) firing levels. Results of firings using well-below-recommended firing levels showed marked increases in delay times above the nominal values. There was also a marked increase in variation, to the extent that out-of-sequence firings would be essentially assured in any typical blasting round at these low firing levels. Within the range of recommended levels the effects of current increases were not considered to be of great importance relative to other overriding effects, such as the significant difference noted in average values of detonators from different lots having the same nominal delay. This effect, when combined with the normal variation noted among members from the same lot, would cause out-of-sequence firings with detonators from a neighboring delay period. Where comparisons with results from another study were possible, it was found that both studies observed quite similar variations in delay times about the average values, and a lower probability of out-of-sequence firings for the shorter delay period groups. The criterion of the previous study for assessing the likelihood of observing out-of-sequence firings, when applied to the Bureau of Mines data, properly identified two neighboring delay period groups where out-of-sequence firings would occur.

Jan 1, 1981

By W. E. Lamont

The Federal Bureau of Mines conducted research to develop methods of removing phosphorus from the earthy, calcareous hematite ores of the Birmingham, Ala., iron district while simultaneously improving the grade and recovery of the iron values prior to furnacing. An attempt was also made to identify the phosphorus minerals present in the ores. The ores contained about 36 percent iron, 12 to 16 percent CaO, 15 to 20 percent hydrochloric acid insolubles, and 0.30 to 0.36 percent phosphorus. Fractions containing 5 to 15 percent phosphorus were isolated from the ores. Collophanite, Ca3P2O3?nH2O, a member of the apatite group, was the only phosphate mineral identified. Beneficiation methods using flotation and reduction roasting with magnetic separation yielded good grade iron concentrates, but were not as effective for reducing the phosphorus content of concentrates. Reduction roasting followed by fine grinding, magnetic separation, and acid leaching gave iron concentrates containing 62.5 percent iron and 0.04 percent phosphorus with an iron recovery of 82.9 percent and a phosphorus rejection of 93.7 percent. Reoxidation of reduced magnetic concentrates followed by acid treatment gave iron concentrates containing 58.1 percent iron and 0.02 percent phosphorus with 89.6 percent recovery of the iron and 96.5 percent rejection of the phosphorus.

Jan 1, 1973

By Dennis R. Dolinar, Eric R. Bauer

Skin failures of roof and rib in underground coal mines continue to be a significant safety hazard for mineworkers. Skin failures do not usually involve failure of the support systems, but result from rock or coal spalling from between the support elements. For instance, in 1997 more than 800 miners were injured by roof and rib falls, of which 98% were the result of skin failures [Bauer et al. 1999]. Also, nearly 80% of the roof and rib failure injuries occurred at or near the working faces in development sections. The face area is a zone where the potential for skin failure accidents and injuries and for roof and rib failures is high because of mining activity, ground readjustment due to changing stress conditions, and the higher exposure of mine workers. In addition, failures occur where the roof and rib are unsupported. This paper reviews the roof and rib accident statistics resulting from skin failure, and highlights the incidences by type, numbers and percentage, in-mine location, supported and unsupported roof, and worker activity at the time of injury. Also discussed are the causes of roof and rib skin failures, current and improved support methods and materials for skin surface control, and machine design modifications for improved roof bolter operator protection. It also reviews the historical literature on skin failures and control methods.

Jan 10, 2000

1.1 Bituminous-Coal and Lignite Dust. - Carboniferous material having a volatile ratio of 12 percent or more by weight and a fineness such that the material passes through a No. 20 sieve. 1.2 Active Underground Workings. - Underground places in which men are required to be or to pass through in the performance of normal mining operations for the production of coal. 1.3 Working Areas. - Underground areas where bituminous coal and lignite are mined, specifically: (a) Face. - The solid surface of the unbroken portion of the coalbed at the advancing end of the working place. (b) Face Area. - The working area inby the last open crosscut in an entry or a room, including the pillar being extracted or longwall being mined. (c) Room. - A place abutting an entry or airway where coal has been mined and extending from the entry or airway to a face. (d) Crosscut (Breakthrough). - Passageways or openings cut through a pillar to connect adjacent entries or rooms. 1.4 Entry. - Underground haulageways, travelways, and airways, except working areas as defined in section 1.3. (a) Active Entry. - An entry in which coal is being mined from a portion thereof or from connected sections. (b) Parallel Entry. - Usually an intake airway parallel to the haulageway. (c) Back Entry. - Usually a return airway parallel to the haulageway.

Jan 1, 1960

By R. H. Nafziger

As part of its program to help decrease the dependency of the United States on foreign imports of nonfuel minerals and to devise technology for the efficient and economic use of domestic resources, the Bureau of Mines smelted and sulfation-leached an ilmenite from northern Minnesota. The objective was to assess the feasibility of preparing chlorination-grade titanium feedstock. The concentrate was smelted with woodchips, coke, and soda ash in 91-kg-and 1-metric ton (mt)-capacity electric arc furnaces to form Ti-rich slag and commercial-grade pig iron. The slag contained from 67 to 77 wt pct titanium oxides and from 1.8 to 7.2 wt pct iron. Sulfation occurred in a 4.5-kg/h moving-bed reactor using S02-air mixtures at temperatures of 8000 to 8500 C to form soluble salts of the Ca, Mg, Mn,and Na impurities, which cause plugging of fluidized-bed chlorinators. Subsequently, the sulfated slag was leached in acid to remove the soluble sulfates. The final product from small-scale testing contained up to 95.5 wt pct Ti02, a minimum of 0.6 wt pct Fe, and a minimum total of 0.3 wt pct of the four impurities of interest. The final product meets charge specifications for chlorination. However, more large-scale testing is necessary.

Jan 1, 1987

By A. L. Johnson

In this Bureau of Mines report, time-resolved infrared emission spectra and corresponding pressure and temperature histories are reported for large-scale propagations of CH4-air, CH4-air-N2, and CH4-air-CF3Br ignitions in a 12-ft-diam sphere. Absolute spectral radiances were obtained throughout combustion over the 1.6- to 4.8-gym range, and the radiance growth patterns for the H20 (2.5-µm) bands are presented as a function of methane stoichiometry and diluent concentration. Flame temperatures were determined from the C02-band emissions, which approximated unit emissivity shortly after ignition. Burning velocities are also given for some of the test-mixture compositions. Measured flame temperatures were in excellent to fair agreement with theoretical adiabatic values for the CH.-air and CH4-air-N2 mixtures; the best agreement was for the stoichiometric CH4-air mixture. The CH4-air-CF3Br mixtures with =2 pct CF3Br gave poor agreement with theory. The measured temperatures were significantly lower during the early stage of combustion; furthermore, the later stage of combustion was uninhibited and yielded unexpectedly high pressures. Supplemental data from a 2-ft-diam sphere at various initial pressures confirmed that the CF3Br inhibition effectiveness decreases with increased pressure. The possible effects of buoyancy, turbulence, and changing kinetics are discussed.

Jan 1, 1977

By A. C. Fieldner

The Bureau of Mires in its investigations of gas masks for use in mines and allied industries has studied and developed various types of masks for protection against noxious uses and furies that may be present in atmospheres encountered in mines, metallurgical works, chemical and other industries. As a result of these investigations, the Bureau issued a schedule5 of tests under which manufacturer who voluntarily submit masks for examination and test, are issued an approval certificate for masks that meet the Bureau's specifications. In the Bureau's schedule, masks arc classified by types of gases removed, as type A masks for protection against acid gases; B; organic vapor; C, ammonia; D, carbon monoxide; E, smoke, dust, and mist; F, special gases; combination types, and type N, for protection in air against all gases, vapors, and smokes. The purpose of this paper is to describe the physical and chemical tests that were conducted on a type N mask, the protective principles and construction of the essential elements of the canister and attachments, and the uses and limitations of this type of mask. The mask tested is known as the all-service mask, manufactured by the Mine Safety Appliances Co., Pittsburgh, Pa;, and was approved (approval No. 1403) by the Bureau on July 1, 1924, for protection from all classes of poisonous vapors, gases and smokes in air.

Jan 1, 1925

By Lisa Steiner, Robin Burgess-Limerick

Working with or near underground coal mining equipment is hazardous because of the multiple sources of energy and adverse environmental conditions. Of the 4169 injuries reported to Coal Services during the three years to June 2005,447 were associated with continuous miners, 232 with LHD (load-haul- dump) vehicles, 140 with shuttle cars, and 140 with personnel transport - a total of 959, or 23% of all injuries reported during the period. An analysis of the injury narratives accompanying these injury claims highlights a number of opportunities for controlling injury risks. Using the frequency of reported injuries for the prioritisation of risk control strategies has limitations because of the tendency to underestimate the importance of relatively uncommon but potentially high consequence events. Injury reports also underestimate the contribution of risk factors such as whole body vibration, which have a long-term cumulative contribution to an elevated risk of injury. However, taking these limitations into consideration, the results of the injury narrative analysis suggests the following hazards as the highest priority for elimination or control: • handling continuous miner cable • strain while bolting • slipping off continuous miner platform • inadvertent or incorrect operation of bolting controls, and operation of controls while a person is in a position of danger • hitting potholes or other roadway abnormality • collisions while driving underground vehicles

By J. Weinberg

This Bureau of Mines report presents data on the changes in the use of steel in motor vehicles over the past 35 yr. Sources of supply of steel for the automotive sector have shifted from almost all domestic in the 1950's to about 50% domestic and 50% foreign in the 1980's. Downsizing, design changes, and substitution of lighter weight materials to achieve energy efficiency also contributed to the market loss of the domestic steel industry. Although plastics and aluminum have displaced some steel in motor vehicles over the years, heavy low-carbon steel is now being replaced most rapidly by lightweight high-strength steel. If the percent of domestic steel used in motor vehicles had not declined since 1950, domestic industry would have supplied 9.3 million more short tons of steel than it supplied in 1985. Downsizing and design changes accounted for 43% of the loss; steel imports, 32%; and substitution of plastics and aluminum, 25%. In 1985, the total value of market share lost by U.S. steel producers was $5.1 billion, of which $1.6 billion was lost to foreign steel producers and automobile manufacturers. Through aggressive marketing and increased efficiency, however, the domestic steel industry may be able to recapture some lost markets, as applications for high-strength steels expand, and as foreign-owned automotive plants in the United States provide fresh sales opportunities.

Jan 1, 1988

By R. Ward Stahl

Fire has been one of man's most useful tools through the ages and certainly is a "must" for industrial progress but when uncontrolled is one of the most destructive agencies. This fact is even more important in a coal mine, where many persons and much expensive equipment are confined in a relatively small area. Means of escape from a burning area, as well as from the products of combustion, are often limited; and in many instances the entire surroundings are combustible. Numerous mine fires, which resulted in a high death toll and great financial loss through the years, have caused mine owners to search for the best fire-fighting equipment; much of this has been installed, the quantity depending largely upon the experience of the individual companies or neighboring mines in certain coalfields. A mine owner or operator has meager published information on the actual fire protection afforded and systems of fire-fighting inaugurated in the coalfields, by which he could compare his efforts and get some idea of the adequacy of his own protection. To further general knowledge of the subject, it was decided to survey a representative number of mines in the field and show what has been accomplished. Representative mines were selected in various coal beds; some had similar tonnage, so comparison could be made if desired.

Jan 1, 1957

By J. W. Thompson

RAILROAD GRANT-MDIERALS. Diatomaceous or infusorial earth when found in such quantity and quality as to render lands containing deposits valuable therefor are mineral lands within the meaning of the mining laws and must be excepted from grants to the Central Pacific Railway Company. Central Pacific Ry. Co., In re, 45 Land Decisions, 223, p. 226. RAILROAD GRANT-CLASSIFICATION, If any evidence of minerals is found upon lands within a railroad grant and the showing is sufficient in the opinion of prudent and qualified persons to warrant further exploration and expenditure, with reasonable prospects of success, then the land can not be classified as nonmineral and is not subject to the grant to a railroad company. But where there is no present indication of minerals nor any geological evidence upon which to base a mineral finding, land should not be classified as mineral, or held for further classification and reserved from the railroad's grant, upon the surmise that future prospects might disclose evidences of minerals. Southern PacUl.c Ry. Co., In re, 45 Land Decisions, 326, p. 329. INDEMNITY SELECTION BY RAILWAY COMPANY, Under section 3 of the act of July 2, 1864 (13 Stat., 365), and the joint resolution of May 31, 1870 (16 Stat., 378), the Northern Pacific Railway Company could take coal and iron land within its primary or grant limits. It could not base an indemnity selection upon the claim that certain land was coal or iron in ;;haracter, as such land was not lost to it as part of the grant. But the company was authorized to select other lands in lieu of those lost because of their mineral character, but the word "mineral" did not include iron or coal, and, accordingly, the railroad company was entitled to take coal lands under its indemnity selection.

Jan 1, 1917

By H. Reginald Hardy

This report describes the results of a research project carried out to investigate the feasibility of using transducer arrays, located on surface or in shallow boreholes, above an active coal mine to detect and locate the source of underground microseismic activity which normally occurs during mining. The initial stage of the project involves the design and development of a self-contained mobile microseismic monitoring facility capable of use in remote field locations. Following this a variety of transducers, and transducer field installation techniques were investigated to obtain optimum sensitivity and high signal-to-noise characteristics. Preliminary efforts were also undertaken to develop semi-automated techniques for analysis of microseismic field data. Using the facilities and techniques developed field studies were carried out at a number of surface locations over a central Pennsylvania coal mine operating at depths of the order of 500 feet. In particular studies were con-ducted over a previously mined development area, troubled by extensive problems of roof instability, and over two longwall panels during mining. Although many of the field studies were carried out during the development stage of the project, results in general have been most encouraging. Limited results were obtained over the development area, however excellent microseismic signals, correlating with underground strata instability, were detected over both long-wall areas, proving the general feasibility of surface monitoring techniques. More recent studies, carried out as part of a subsequent project, and utilizing modified geophone installation techniques at a third longwall site, have verified explicitly the feasibility of measuring underground microseismic activity from surface locations. Sections of typical field data are included in this report along with a brief review of the studies carried out at each of the field sites. Detailed analysis of data obtained at the second and third longwall test sites will be presented in a later report.

Jan 1, 1974

By Richard L. Fowler

Study and development of sensing techniques and sensors were performed to aid shuttle car drivers in detecting obstacles and in guiding the car along the face haulage route. Microwave, acoustic, and optical sensing techniques were considered as part of the feasibility study for obstacle detection. Various guidance techniques, including wire-following and rib-ranging were investigated. Active optical sensing was selected for obstacle detection to obtain the beam coverage and sharp angular cutoff characteristics required within the packaging limitations defined by the shuttle car configuration. Rib-ranging guidance was selected to achieve a completely self-contained shuttle car system which responds to the existing mine geometry without need for wires, stripes, or other path defining devices. Extensive hybrid computer simulation runs were performed to evaluate various guidance techniques during the feasibility study. Subsequent simulation runs were performed to establish parameter values for the rib-ranging guidance system. The obstacle detection and guidance system was designed, fabricated and installed on a standard shuttle car. The system satisfied all applicable permissibility requirements of Schedule 2G. An experimental permit was issued to Bendix for operation in an underground coal mine. System evaluation tests were performed first above ground at the Bendix Research Laboratories. The simulation model was validated by these runs. Final testing was performed underground in an operating mine with an experienced shuttle car driver. All sensors successfully demonstrated the predicted performance capability during underground face haulage tests. Dust did not impair system performance and lens cleaning was not required during working shifts. Further development is required to achieve the desired obstacle detection performance. Closed loop steering control with manual override is recommended for the lateral guidance system. The guidance system should be an invaluable aid to low-coal shuttle car drivers where continuous mining machines are utilized.

Jan 1, 1973

By T. E. Howard

The western phosphate field, comprising parts of Idaho, Montana, Wyoming, and Utah, contains one of the world's largest known reserves of phosphate rock. Although phosphate-rock deposits of good-grade have been known since before the turn of the century and production has been recorded since 1906, real development of this important field did not begin until immediately after World War II. Since then fertilizer-manufacturing facilities using western phosphate rock have been expanded, and three electric-furnace plants for producing elemental phosphorus have been installed, resulting in a rise in mine production from 323,955 long tons2/ in 1945 to 1,653,916 long tons3/ in 1953. Interest in the field is increasing, and it is reasonable to expect that the western phosphate industry will continue to expand. Before 1945 all western production was from underground mines. In that year the first strip mine in the field was started near Montpelier, Idaho,~ and in sub-sequent years a number of other open-pit mines were opened in southeast Idaho and western Wyoming. At present the major part of the production comes from surface mines. Underground mining has continued, and new underground mines have been opened in the field, but recent exploration by operating companies has been aimed primarily at developing additional deposits suitable for low-cost surface mining. Preliminary reserve estimates by the Federal Geological Survey5/ indicate that only a very small part of the total resource may be recovered by surface methods and that the industry eventually must depend largely on underground mining. Because one function of the Bureau of Mines is promoting the conservation and development of the Nation's mineral resources, it is appropriate that research be conducted to develop low-cost maximum-recovery underground mining methods applicable to western phosphate-rock deposits.

Jan 1, 1956

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

"Investigations in the Federal Bureau of Mines Experimental coal mine near Pittsburgh, Pa., have shown that high-expansion foam containing at least 0.2 ounce of water per cubic foot of volume is effective in controlling exper-imental underground coal, oil, or wood fires. Some of the fires were extinguished, but more of the coal and wood fires were brought under enough control to permit direct attack with water or other extinguishing agent or loading the hot material into cars. The largest controlled experimental fire, which burned about 5 hours before attack, was in a coalbed 5 feet wide, 10 inches thick, and 100 feet long. The greatest distance foam was transported to control a fire was 1,010 feet.An incipient fire should be attacked promptly with water, rock dust, or other approved and readily available extinguishing agents. Where heat, roof falls, and smoke prevent direct approach, the more involved procedure of using foam may be advantageous. The effectiveness of the foam in controlling a deep coated fire of considerable extent H,vet to be proved by actual trials in aSome hydrogen, carbon monoxide, and methane gases are generated when a fire is attacked with foam. Calculations showed that in experimental fire tests an explosive mixture could form; however, this would occur only within a narrow range of combustible gas-air mixtures not likely to be found in practice. The principal explosion hazards are due to generation of gases by the foam, localized build-up of normally liberated methane, and volatiles liberated by the coal during heating. The quantity of combustible gases generated by the action of the foam on the fire is about the same as that when an equivalent amount of water is applied."

Mar 1, 1960

By Irving Hartmann

Several recent ignitions of firedamp - a mixture of methane and air - in American coal mines have been attributed to frictional heating when hard rocks were struck while cutting and drilling coal seams. Although none of these ignitions caused severe explosions, they call attention to a problem that can become increasingly significant as mechanized mining is developed further. The power in and rapid release of energy from high-speed machinery has increased the rates of advance into virgin coal creating many problems. Unforeseen faults and hard mineral inclusions may be encountered; coal brought down in this way is finer in size; more gas is released from the seam; it is frequently more difficult to provide adequate ventilation at the' face; and new roof-support problems must be solved. In particular, continuous mining machines (also known as continuous miners) greatly increase the frequency of contact between cutter bits and minerals. In view of these conditions, it may be expected that more gas ignitions will occur as a result of frictional heating unless the situation is understood and remedial measures are introduced. The problem of frictional heating is not new in coal mining. In Europe, particularly in England, it has been a concern for more than a century. During the last 15 to 20 years frictional ignitions have been a major cuase of explosions in British mines. Explanations for the greater number of such ignitions in England may be the special character of the coal measure strata, the mining methods, the rate of gas emission and possibly its composition, and less effective ventilation near the face. To reduce the ignition hazard, considerable laboratory and field research has been conducted, particularly by the Safety in Mines Research Establishment, Ministry of Fuel and Power of Great Britain. Much of the information presented in this report has been drawn from these studies.

Jan 1, 1955

[This Report represents the culmination of work perfomed under Contract No. .,JG1551A8 for the U.S. Bureau of Mine.The &apos;.:o-< embeded a site evaluation, engineering E:-y- ,, esign, and preparation of specifications for construction of a Transport Research 7 :4 (HTRF)The HTRF is designed as a research facility J evaluate the hydraulic transport of large lump coal at a prototype ;e scale. The HTRF is to be constructed and operated by the Pittsburgh and Safety Research Center of ;. re U.-AN a*, their Bruceton, Pennsylvania test center. In terms of technical capability, the HTRF will have transport pipeline:: of -, twelve-, and eighteen-inch diameter _&apos; with supporting coal handling n , water forage a.^ &apos;d conveyance, mixing, pumping, and dewatering equipment, plus instrumentation and controls. Maximum design velocity 13 20 ft/sec.; solids concentration, by, volume, will; 1 be a maximum-- of sixty, percent. Each test loop is designed to accommodate solids of up to one-third the diameter e - of the pine. The Final Report Pr.-&apos;I-rents information of t HTHF,. including the site evaluation, design criteria, a description of the a description of the procedure to be used for operation of the facility, an estimate of the cost to construct the f^Cilit:r, 1 p el_~lli.&apos;iU construe`, icn Schedule, and a construction suicJ_iicaT.l_ccn&apos;. T e c011SLr?Jc&apos;.ion soecl_ i.on _ccnta_i:s technic.&apos;..i re7,uir: (-n`,s for !&apos;urr1S~ &apos;~latcr..al. and ec-uipr,ent for :":C1 C_`:_C ti on of ti,_ H ice&apos; u:&apos;.:i ._II u s(-.6 for ~.Iir: .3!7 soliciting bids. `.l_o included n cc&apos;;,art_- c?r~.air sV:et..: :s ^nd rr^.?]

Jan 1, 1976

By R. Hogg, T. F. Dumm

"It is generally agreed that dust characteristics play a role in the development of Coal Workers' Pneumoconiosis (CWP). Unfortunately, there is a serious lack of information on what the characteristics of mine dust actually are and how they vary among different mining regions, coal seams, etc. This paucity of data can generally be attributed to the serious problems encountered in collecting sufficiently large quantities of dust for conventional analytical procedures.Personal samplers are widely used in coal mines for regulatory and enforcement purposes. Generally, these provide information only on the total (respirable) dust loading in the mine atmosphere and on the mineral matter (primarily quartz) content of the respirable dust. A procedure has been developed by which samples collected with a slightly modified personal sampler can be analyzed for particle size distribution, total mineral matter content and elemental composition, in addition to the standard mass and quartz measurements. These analyses could readily be performed on a routine basis. Shape analysis by Scanning Electron Microscope (SEM) could easily be included if appropriate shape criteria are established. Extension of the procedure to include the determination of complete size/specific gravity (composition) distributions is quite straightforward provided sufficiently large samples (at least 10 mg) can be collected. Typical sample sizes for a personal sampler carried by a miner for one shift range from about 0.5 to 2 mg.The basic procedure was developed and evaluated using synthetic mine dust prepared in the laboratory. Field tests in three working mines in Pennsylvania and West Virginia have confirmed the applicability of the approach to the real world. Particle size distribution measurements on mine dust collected in the modified personal sampler were found to agree closely with the results of simultaneous in situ measurements obtained using cascade impactors."

Mar 1, 1989

By C. H. Fisher

Sulphuric acid of various concentrations has long been used as a reagent in the determination of olefins and aromatics in hydrocarbon oils4 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 80 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 sulphoric acids being considered as saturated hydrocarbons. In some cases the saturates are examined further by differentiating between 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.

Jan 1, 1937