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By L. C. IlsLey

The Bureau of Mines has collected field data and made laboratory investigations of trailing- cable performance in the hope of developing a better and safer cable for use with permissible mining machines . Because of their better insulation and performance , only rubber- sheathed cables were finally considered . The cables tested represented the product of six manufacturers . : After consideration of the results of the preliminary investigations , the conditions under which cables are used in mines , and the better performance of the later types of cables that were submitted as the investigation progressed , the bureau formulated a performance - test requirement and notified the cable manufacturers as follows : The hazards of the trailing cable are such that the bureau has been unable to extend beyond the machine its formal approval to cover the cable as at present developed . However , in the attempt to reduce the hazard as much as possible , cables passing certain tests will be recommended for this service and it is hoped that several cables will be developed to meet this requirement .

Sep 1, 1930

By Thomas M. Barczak

The transverse loading requirement for stoppings as specified in the current Code of Federal Regulations is 39 psf. This measure is based on physical testing of a freestanding wall in accordance with ASTM E 72 specifications, where the dominant parameter is the tensile strength of the sealant. A new protocol based on arching has been developed to determine the true transverse load capacity of stoppings. Arching is achieved by the restraint of the stopping against the mine roof and floor, whereby compressive forces are developed within the wall. A laboratory procedure using the NIOSH Mine Roof Simulator (MRS) to simulate rigid-arching of stoppings was developed and verified through full-scale in-mine tests. Using this protocol, a systematic study of the design parameters that affect arching capability in block stoppings was conducted. The study included a theoretical assessment of arching and development of design formulations that can accurately define the transverse load capacity of various stopping constructions under various loading conditions. This approach should lead to a safer mine environment by matching the transverse load capabilities of the stopping design to the requirements in the mine to ensure proper ventilation control is maintained.

Jan 1, 2005

By Lisa Steiner

Almost every process has a predecessor, and studying the predecessor helps to define needs and shortcomings to be addressed in the new design. It also suggests what information is needed by the users in order for them to be able to operate safely and effectively. The end users of a system can provide important feedback to better evaluate the current and proposed designs. When new technology is introduced into a system, mishaps may occur before it is realized that human-system interactions were not considered adequately in the design process. A systematic methodology to evaluate the causes of these injuries and to develop remedial recommendations can enhance safety. This paper illustrates how such an approach was used to assess remote machine operation in underground coal mines. The dynamic work environment of underground mining with its unpredictable geologic anomalies can result in numerous hazards. Many of these hazards, including mine roof collapse, occur near the working face where coal is being extracted. The face area is also where the most intricate interactions of people and equipment occur. For these reasons, a high priority has been placed upon minimizing hazards to the workers at the face. A remote control operation was introduced to provide a safer working distance from these hazards. As the remote control technology began to be widely used for extended cut mining operations, new issues became evident. It was essential to develop mechanisms for mines to evaluate these issues in order to predict and reduce injuries. Mining methods and equipment changes must allow for the ability of workers to adapt to changes in their dynamic mining environment. Consideration should be given to how the worker will use familiar information to make decisions in now unfamiliar situations. There will be both intended and unintended consequences [Merton, 1949]. Designers try to anticipate and eliminate surprises, but it is impossible to eliminate them all. How, then, will the new system affect the tasks to workers which are currently accustomed? As suggested below, this question may be addressed and more of the unintended outcomes predicted with a planned design process which includes strong human factors input to determine interactions and behaviors of participants.

Jan 1, 2005

Reduce the potential of haulage related injuries in underground mines by providing a method for quickly assessing the state of repair of mine haulage track. The Problem Currently, there are no established standards or procedures for inspection or cleaning of underground mine haulage track. Many track defects are hidden from an inspector because of layers of dirt and debris on the ballast, spikes, fishplates, etc. When a visual inspection can be performed, it may be highly subjective, except for a few items that can be categorized or counted, such as missing bolts or spikes. Track inspectors may even become tolerant of defects that can gradually worsen. For these reasons, mechanical inspection methods are needed to supplement visual inspections. Approach The Bureau investigated this problem and designed a towed vehicle to both mechanically clean and inspect underground coal mine haulage track. The vehicle was developed using a systems approach, paying particular attention to human factors issues such as operator field of view, operator ingress-egress, control positioning, and seating design. The prototype was built using simple fabrication techniques and off-the-shelf components.

Jan 1, 1990

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 Peter G. Kovalchik, Lawrence W. Scott, Thomas H. Dubaniewicz, Frank T. Duda

Overheating of electric cables on shuttle cars has long been recognized as a cause of premature insulation failure leading to shock and electrocution. Use of cable reels on shuttle cars can cause excessive heat build up which, in turn, causes the cable insulation to soften and become easily damaged This heat-softened insulation reduces the life of the cable. Repeated cycling of a cable in this manner can cause premature aging of the insulation; it becomes bridle, cracks and allows electrical leakage paths to farm. These leakage paths provide the opportunity for shock and electrocution to occur if miners come in contact with the damaged section of cable. It is imperative that cable operating temperatures be maintained at safe thermal limits. This paper discusses a research project conducted by the National Institute for Occupational Safety and Health, Pittsburgh Research Center to determine dynamically the conductor temperature of reeled shuttle car cables using fiber optics technology. The research portrays typical shuttle car loading cycles (both current and time cycles). Root-mean-square current loading is calculated based on the results. The thrust of this effort is to provide the scientific basis for ampacity derating factors specifically for mine machinery using reeled cables This information will reduce the probability of electrical hazards from reeled cables

1. In 2002, a total of 2,065 coal mining operations reported employment to the Mine Safety and Health Administration (MSHA). Coal mines comprised 14.2% of all mining operations. • Bituminous mines comprised 92.5% (n = 1,910) and anthracite mines 7.5% (n = 155) of coal mining operations. • More than 70% of all coal mines were located in three states: Kentucky (28.7%), West Virginia (21.7%), and Pennsylvania (20.1%).

Jan 1, 2004

By William H. Pailes, Vincent Castronova, Daniel Lewis, Norman L. Lapp, George Goodman

"INTRODCJCTIONAlveolar macrophages are free lung cells located on the surface of small airways and alveoli. These phagocytes play an important role in the protection of the lung against airborne bacteria and particles.1 However, hyperactivation of pulmonary phagocytes can lead to excessive secretion of enzymes and reactive oxygen species which could result in lung injury, emphysema, or fibrosis.2,3 Analysis of bronchoalveolar lavage effluents for cell types and cellular activity has yielded information concerning the etiology of various pneumoconioses. For example, emphysema associated with inhalation of coal dust or cigarette smoke has been related to enhanced secretion of reactive oxygen species from alveolar macrophages.4-7 In contrast, hypoactivation of alveolar macrophages has been associated with inhalation of diesel particulates"" and has been related to increased susceptibility to pulmonary infection. s Inhalation of cotton dust has been associated with dramatic increases in lavagable polymorphonuclear leukocytes9 while pulmonary sarcoidosis and silicosis have been related with high numbers of lymphocytes in lavage effluentsl0,11The objective of the present study was to obtain lavage effluents from 8 control subjects, 8 healthy power plant workers exposed to fly ash, 1 healthy coal miner, and 1 rock driller with acute silicosis. These effluents were analyzed for total numbers of alveolar macrophages, lymphocytes and neutrophils and for secretory activity of alveolar macrophages. Data were then analyzed to determine what response patterns were characteristic for given dust exposures.METHODSSelection of SubjectsThe 8 control subjectS were all adult males from the area of Morgantown, WV. Two subjects among the controls had smoked cigarettes for approximately three pack-years and had stopped more than ten years ago. The 8 power plant :workers were all healthy adult male employees of a power facility in Hatfield, PA, approximately thirty miles from Morgantown. One of the power plant personnel was a comparable ex-smoker. The remaining subjects were all lifelong non-smokers. The coal miner was a healthy non-smoking male from Morgantown, WV. The rock driller was a patient under treatment with corticosteroids for acute silicosis. He had shown considerable clinical improvement with this treatment but still manifested significant radiologic and pulmonary functional abnonnalities at the time of lavage. The mean age of the 8 control subjects was 36 years (range: 31 to 49 years); the mean age of the remaining subjects studied was 38 years (range: 29 to 53 years)."

Jan 1, 1990

By John A. Organiscak

Enclosed cabs are a primary means of reducing equipment operators? silica dust exposure at surface mines. The National Institute of Occupational Safety and Health recently performed a laboratory study to evaluate which factors on an enclosed-cab filtration system are most significant. The various factors evaluated were intake filter efficiency, intake air leakage, intake filter loading, wind infiltration, use of a recirculation filter, and the use of an intake pressurization fan. The result of this laboratory testing has shown that the two most important factors for an effective filtration system on an enclosed cab were the efficiency of the intake filter and the use of a recirculation filter. A higher-efficiency intake filter considerably increased the quality of the intake air that was delivered into the enclosed cab. It also was determined that air leakage around the intake filter notice-ably reduced its air cleaning effectiveness. The second key factor is the use of a recirculation filter, which was shown to improve the air quality in the enclosed cab by six to 12.7 times more than the intake filter alone. The reason for the significant improvement was that the cab air was constantly drawn through the recirculation filter, thus continually filtering the dust out of the air.

Jan 1, 2010

By F. S. Crawford

Untreated timber in a mine or elsewhere may fail prematurely because it may "rot out before it wears out." If such timber is treated with a satisfactory preservative, decay will be retarded for many years, and it's serviceable life will beg prolonged to several times that usually obtained from untreated timber.4/ Treated timber has many advantages, and although it has been used extensively by railroads and other large consumers of structural timber, the relatively small use in mines seems strange indeed. Timber does not decay if it is kept dry, cool, and well-ventilated or if it is kept constantly wet or sumberged in water. At a mine in Canada the temperature in the upper levels was only 44° F., and the timber did not decay. As operations deepened, however, warmer ground was opened, and, with high humidity, conditions favored timber decay. The life of untreated timber may be only 2 to 3 years under such conditions.

Jan 1, 1951

By H. B. Freaman, C. L. Colburn, C. M. Bouton

"The mine telephone has been perfected to such an extent that it is giving satisfaction in most mines were the wiring is well insulated. Very often the telephone cannot be depended upon on account of falls of rock, grounding due to worn insulation or extreme dampness. In the event of a disaster it frequently happens that the mine telephone system is put out of commission by the agency that causes the disaster, at the time when it is most urgently needed. On this account the mining industry is interested in any kind of telephone system that can be counted upon in an emergency. Many requests have been received by the Bureau of Mines to devise means of utilizing wireless methods for this purpose.The results of some preliminary experiments conducted by the writers at the Bureau of Mines experimental mine at Bruceton, Pennsylvania, in the ordinary sending and receiving of radio waves through earth strata are described below. The experiments were made in cooperation with the Westinghouse Electric end Manufacturing Co., which assigned to this work three of its radio engineers, C. A, Boddie, E. C. Douglas, and F. D. Fessler,The preliminary experiments consisted first in receiving signals from without the mine by means of a receiver located inside the mina, and second, both sending and receiving messages underground through the strata. It was found that with a receiving instrument set at a point 100 feet underground, signals from KDKA station, of the Westinghouse Electric and Manufacturing Co. East Pittsburgh, Pa., could be heard distinctly. Station KDKA is at a distance of about 18 miles from the experimental mine. About 50 feet from the receiving station used in this test was a 6-inch bore-hole from the surface, lined with iron pipe and containing electric light wires which extended therefrom through-out the mine. The presence of these wires evidently assisted greatly in the reception, for when the receiving set was carried to another point in the mine removed from wires and tracks the signals were barely audible through 50 feet of cover. The fact that signals were detected, however, even though faintly, is sufficient evidence of transmission through the ground to encourage further experimenting.In sending waves underground the Westinghouse 20-watt B.T. model T.F. transmitter was used in such a manner as to send out continuous waves of 200 to 300 meters length."

Oct 1, 1922

By A. B. Hooker, J. W. Paul

"There was a time when any suggestion that the Davy flame (safety) lamp be discarded, would have evoked unlimited, criticism. However, that time is past.Investigations both here and abroad have shown conclusively that the Davy lamp does not have the necessary factor of safety against ignitions of mine gas, and England, the lost stronghold of the Davy lamp in Europe, has eliminated this lamp and substituted safer types.In the United States there are companies who still use the Davy lamp in spite of all that has been said and published as to the dangers connected with its use.Recently the purchasing agent of an anthracite coal company requested the Department of the Interior, Bureau of Mines, to pass upon the safety of some braise gauzes for use in a shielded Davy lamp. A shielded Davy lamp is an ordinary Davy safety lamp equipped with a circular brass shield that is attached to the lamp posts. This shield extends about one-half way around the gauze and one-half of the gauze height. The main purpose of the shield is to prevent the lamps being extinguished by a sudden increase in the velocity of the air current past the lamp.The brass gauzes submitted for this test represented two grades of brass - a yellow brass and a red brass. The analysis of these brasses was not determined. Two shielded Davy lamps that were submitted for the tests each had a steel gauze. These steel gauzes were also tested. Tests were made in horizontally moving mixtures of Pittsburgh natural gas and air at velocities of 400 to 1,000 feet per minute. The gas percentages used were 7%, 8.6%, and 11%. Tests were made with the lamp shield in two positions relative to the lamp and direction of flow of the gas-and-air mixture. In one position the shield was between the gauze and flow, as normally used. In the other position the shield was on the downstream side of the lamp. The tests were continued until one or more failures or gas explosions been obtained with each of the six gauzes. The results of these tests summarized as follows:"

Jun 1, 1923

By Richard J. Mainiero, Harry C. Verakis

The Bureau of Mines has conducted research to determine whether the total elapsed delay time for blasting bituminous coal in underground mines could be safely expanded beyond the present 500-ms limitation without igniting a methane or methane-coal dust atmosphere. The results indicated that the increase of total delay from 500 to 1,000 ms had no detectable effect on safety relative to incendivity as long as permissible practices were observed in all other aspects. Research was also conducted to evaluate the safety of 18-in hole spacing for delay blasting in coal relative to misfires. For a variety of permissible explosives, misfires were observed for about 50 pct of the holes at 18-in spacing. Based on this observation, the Bureau has recommended that the new regulations prohibit hole spacings of less than 24 inches in underground coal mines. Misfires were also observed for 24-in spacing, but the number of misfires and test shots was too small to sup- port any firm conclusions.

By Alfred R. Powell

In another paper the writer has described an investigation in which the forms of sulphur in coke were determined and described. Coke was found to contain four characteristic forms of sulphur- namely, ferrous sulphide, sulphates, ad- sorbed free sulphur, and sulphur held in solid solution in the carbon. While the coke is still in the oven, only two forms of sulphur are present namely, the ferrous sulphide and the sulphur in solid solution in the carbon. During the quenching, however, the sulphur of the coke is subjected to considerable oxidation, a portion of the ferrous sulphide being oxidized to free sulphur and sulphates, while the solid solution form remains unchanged. The coke, however, loses no sulphur during this process, since the free sulphur which is formed ie retained by the coke in an adsorbed form. Since this oxidation of the ferrous sulphide took place so easily, an inves- tigation was undertaken to determine whether this property could not be taken ad- vantage of in some industrial process for the desulphurization of coke. Although it is true that such a roasting process would not touch the solid-solution form of sul- phur, still the removal of the ferrous sulphide sulphur would undoubtedly benefit the coke from the standpoint of the metallurgist. This improvement in the coke would result not only from the decrease in total sulphur, but also from the large decrease in the ferrous sulphide, which is responsible for the contamination of the iron in the upper part of the blast-furnace. The de sulphurization of coke by roasting in air it a new idea, but dates back to the earliest days of coke manufacture. In 1871, Philipparts published the results of some work done by him on the de sulphurization of coke by air, as well as a review of the results of earlier investigators. In the se earlier experiments, nothing was known of the forms in which the sulphur existed in the coke, while the temperature measurements were only approximate, so that altogether the results were not very conclusive nor complete. The de sulphurisation figures given by the se early investigators generally showed a low efficiency for the process, but some extraordinary results were claimed by certain inventors. In the light of our new knowledge concerning the coke sulphur, it seemed to be important enough to warrant investigation.

Apr 1, 1923

Develop a reliable, portable device for non-destructively testing the support integrity of a friction rock support (commonly referred to as a Split Set ). Approach The friction rock support, used to support mine roof and ribs, is a slotted tube driven into a drilled hole of smaller diameter. Upon installation, the tube is compressed radially. The amount of compression is a function of the hole diameter, the strength of the host rock, and the properties of the split set itself. A simple lightweight self-contained device was developed to determine the pull-out resistance of the friction rock supports in-situ, based on measurements of the tube's deformation. The tester measures the com-pressed internal volume of the slotted tube, which has been found to provide an estimate of the support's resistance to pull out. How It Works The tester consists of a pump and expander sections. The expander sections are made from an elastomer membrane which is stretched over two cores, each one inch in diameter and twelve inches long. The expanders are connected by a flexible coupler so that they can fit any alignment of the support.

Jan 1, 1984

By H. J. Heinen

This report summarizes preliminary research studies by the Bureau of Mines in electrowinning molybdenum directly from pure or impure molybdenum trioxide (MoO3) by fused-bath electrolysis in an open graphite cell without need of a protective inert atmosphere. A formulated electrolyte of the tertiary system containing 41.6 percent sodium pyrophosphate, 16.7 percent sodium tetraborat, 33.3 percent sodium chloride, and 8,4 percent molybdenum trioxide, by weight, electrolyzed at 1,000° C,, gave excellent results. Current density studies were made over a range from 20 to 260 amperes per square decimeter. Current efficiencies of 80 to 90 percent were obtained over the entire range. Yields up to 500 grams of molybdenum per kilowatt-hour were obtained. Higher current densities, however, reduced yields and produced a finer grained metal. The two most important facets in electrowinning molybdenum from MoO3, in an open cell, are temperature and electrode spacing to minimize or eliminate the formation of the suboxide MoO2, the major source of oxygen contamination. At temperatures of 1,000° C. and higher, together with the proper spacing of the electrodes, formation of oxides are practically eliminated. Molybdenum metal electrowon from pure MoO3 was 99.9 percent pure and contained 0,056 percent oxygen and 0,007 percent carbon. This metal, when arc-melted, had a Vickers hardness number of 175 and contained 50 parts per million oxygen and less than 10 parts per million carbon. Molybdenum metal electrowon directly from an impure MoO3 containing 90 percent MoO3 resulted in a metal of 99.8 percent purity.

Jan 1, 1961

By B. J. Moore

This Bureau of Mines publication contains analyses and related source data for 276 natural gas samples from 23 States. All samples except four were collected during calendar year 1984. Those four samples were collected earlier, but releases granting permission to publish were not received until 1984. All samples were obtained and analyzed as part of Bureau of Mines investigations of the occurrences of helium in natural gases of countries with free market economies. This survey has been conducted since 1917. The analyses published herein were made by the mass spectrometer and chromatograph. The results of these investigations are published annually to make the information available to the petroleum industry and the general public. Twenty-eight publications have presented the results of 13,957 gas analyses made prior to 1984. The first three bulletins (1-3)2 contain analyses and related source data on 5,218 gas samples collected from 1917 through 1960; these bulletins have been supplemented annually by information circulars (4-17, 19-24, 26-28) containing 8,453 analyses of samples collected since 1960.

Jan 1, 1985

Although the Stamler feeder/breaker has been used for coal crushing in underground mines for many years, it has only recently been applied to other crushing operations. Two companies presently using Stamler feeder/breakers for rock crushing were contacted regarding their experiences with the units in actual field use. In both cases information was obtained directly from the individuals responsible for field operation and maintenance of the units. White Pine Copper Co. has been using Stamler feeder/breakers for over two years to crush copper ore. They now have fourteen 450-ton-per-hour units on line. The ore has a compressive strength of from 18,000 to 28,000 psi and is extremely abrasive. Maintenance is performed on a tonnage basis. The breaker shaft is replaced every 250,000 tons (requiring about 4 hrs) and picks are replaced about every 1500 tons by the operator (requiring about 2 min per pick). Very little unscheduled maintenance has been required. Crushing costs are fairly high (estimated at 13 to 15t per ton including maintenance and operation) because of tale extreme abrasiveness of the material. A new Stamler feeder/breaker with Ultramet wear surfaces was put or line in June 1976. Ultramet was found to increase the life of belt transfer station surfaces by up to 400 percent and it is hoped that it will do the same for the feeder/breaker. At this time it is still too early to evaluate the performance of the Ultramet unit. If it does improve abrasion resistance, crushing costs could be greatly reduced. White Pine is very pleased with the units and the service provided by Stamler.

Jan 1, 1976

By N. T. Lowe, R. E. Miller

When two pieces of heavy equipment interact, jolting and jarring can occur. During haulage truck loading for example, there is a chance that the operator of one or both pieces of the equipment will experience jolting and jarring. Additionally, a jolt can occur when an off highway equipment operator drives over a road defect or inadvertently strikes a berm. Aside from the operators, there is seldom anyone else that witnesses the interaction and can accurately describe the extent of the jolting. This makes it difficult for health and safety managers to address jolting and jarring. The devices and software described in this paper constitute a method for installing “black boxes” called Shox Boxes onboard equipment that already have a GPS system onboard. The resulting configuration provides an objective assessment of jolting and a chance to determine the root causes of it. The Shox Box system reviews data in real time, onboard the vehicles, 24 hrs a day, and sends pertinent information via radio to a central database. The data generated shows whether jolts are above or below a supervisor defined target value for the equipment and the tasks being performed. This allows health and safety personnel to demonstrate safe operation of heavy equipment and recommend proactive actions to maintain jolting within a reasonable range.

By Harry Freund, Kenneth H. Hammill, Francis C. Bissonnette

"Gallic acid is a sensitive, stable, colorimetric reagent for the determination of tantalum in the range of 2 to 40 µ g.Ta/ml. The method consists of the fusion of tantalum oxide with potassium pyrosulfate and solution of the cooled melt in saturated ammonium oxalate, followed by development of a yellow complex with an ethanolic solution of gallic acid. The tantalum-gallic acid complex absorbs over a broad region in the blue and near ultraviolet. Adverse effects due to interfering ions and solution conditions, such as oxalate concentration and pH, can be minimized by a suitable choice of wave length.by a suitable choice of wave length.A new and sensitive colorimetric method is provided that has been used successfully at the Northwest Electrodevelopment Laboratory of the Federal Bureau of Mines for determining minor amounts of tantalum.INTRODUCTIONThe development of corrosion-resistant alloys at the Northwest Electrodevelopment Laboratory prompted a review of the analytical chemistry of columbium (niobium) and tantahnn. Not only are these elements difficult to determine in small amounts, but tantalum especially lacks both sensitive and characteristic color reactions. Various phenolic compounds have been suggested as colorimetric reagents for tantalum, Quentin and Wagner (10, p. 24B) 1/ recommend the use of tannin. The use of pyrogallol was suggested originally by Krivoshlykov (6, pp. 59-60), whose method recently has been subject to a number of modifications (3, pp. 249-254; 5, pp. 1340-1344; 1, pp. 1803-18oi; 4, pp. 345-350). The yellow coloration produced by pyrocatechol in an oxalate solution containing tantalum may also be used to estimate tantalum ( 11, pp, ll-1-4-148) . The use of hydrogen peroxide has been recommended also (7, pp. 164-165; 9, pp. 926-931).Aside from a lack of specificity and sensitivity, the major failing of phenolic reagents is their susceptibility to air oxidation. The oxidation products are highly colored and absorb in the same spectral region as the tantalum complex. Holding reductants are not completely satisfactory in minimizing this effect. Increasing the acidity, while retarding the oxidation, has an adverse effect on the tantalum sensitivity."

Sep 1, 1956