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By S. J. Hussey

This Bureau of Mines report presents a discussion of the statistical approach to the design of experiments and indicates, by concrete examples, how and when statistical design is essential for obtaining meaningful data with a minimum number of experiments. Every research worker plans his work and designs his experiments in a manner which, based on his experience, seems most rational to him and which he believes will produce the information essential for resolving the problems. If the results obtained are open to multiple interpretations and are not of definitive reliability, the failure of the experiment design to produce the desired information may be due to several causes, These include faulty judgment in selecting the factors to be tested, ignoring the importance of interaction between factors, failure to adequately control test variables, and assuming that meaningful trends in the results can be identified without comparison to a predetermined experimental error. An experienced researcher probably will deduce from the nature of the data obtained that the design is faulty and may by trial and error ultimately arrive at the correct solution to the problem. Statistical methods of planning research minimize the chance of faulty experiment design, embody concrete procedures for testing the validity and reliability of the test data and for indicating mandatory changes in the design, and enable the researcher to obtain meaningful information with the least number of tests.

Jan 1, 1963

By Robert C. Johnson

Water-swelling fluormicas and fluormontmorillonoids were synthesized and described. They were found predominantly in the system Mg0 - MgF2 - Si02, with varying amounts of Li+ or Na+, Some water-swelling synthetic minerals were prepared with only strontium or lead in the twelvefold position, Water- swelling compounds containing either K+ or Ba+ were not found. The synthesized water-swelling products were shown by electron microscopy, X-ray diffraction, and chemical analysis to be typically two-silica-layer, platy compounds, Except for the complete substitution of fluoride for hydroxyl, the compounds were similar to the natural micas or montmorillonites. The stability and properties of the compounds were further established by electrodialysis, by differential thermal analysis, and by anion and cation exchange methods. Fluoride in the interlayer positions was nonexchangeable except through decomposition of the product. Exchanging the sodium or the lithium of the synthetic fluormicas or fluormontmorillonoids with potassium ion, particularly those derived from KOH provided a product from which a completely inorganic paper of extraordinary flexibility was fabricated. This paper had excellent mechanical and electrical properties except for water adsorption and a high power factor. Neither of these problems was solved during this investigation. However, papers with dielectric strength from 1,500 to 5,000 volts per mil were readily fabricated, particularly from the lithium containing fluormicas or fluormontmorill onoids.

Jan 1, 1963

By Robert S. Warfield

The Bureau of Mines investigated a geologically favorable area in the Beluga River coalfield in south-central Alaska to determine if there were sufficient minable coal reserves for onsite utilization to meet the projected thermal power needs of the Anchorage area. A program of diamond core drilling and sampling delimited a shallow saucerlike structure estimated to contain indicated reserves of more than 20 million tons of subbitminous coal in a seam over 50 feet thick that could be mined by opencut methods. A large sample of fresh coal was taken across the full width of the seam for washability studies. This sample, with 4 volume-percent of clay partings eliminated, contained 24.4 percent moisture and 16.8 percent ash and had a calorific value of 7,162 Btu per pound. The studies indicated that mechanical cleaning would be of doubtful value.

Jan 1, 1963

By L. J. E. Hofer

This Bureau of Mines study, part of a broad program of research in air pollution related to minerals, was conducted to determine the nature and extent of the poisoning of catalysts when used to remove certain air pollutants from exhaust gases. The poisoning examined in this investigation occurs when leaded gasoline is used as a fuel for automotive engines. This research was conducted in cooperation with the Public Health Service. The smog in the Los Angeles area is attributed to the effect of radiant energy on the mixture of hydrocarbons and nitrogen oxides found in the atmosphere there. A large portion of the hydrocarbons is believed to originate in the exhaust gases of automobiles. To prevent the escape of these hydrocarbons into the atmosphere catalytic mufflers have been proposed. In principle, these are simple and nonmechanical, consisting of a vessel charged with a catalyst capable of destroying the exhaust hydrocarbons by catalyzing their oxidation. However, these catalysts are severely affected by the particulate matter, mainly in the form of lead sulfate (PbS04), lead oxysulfate (PbS04.Pb0), and Lead chlorobromide (Pb(Cl,Br)2), contained in the exhaust gas. Deposition of lead on the catalyst as PbS04, PbS04, PbS0, and Pb(Cl,Br)2 restricts catalytic activity. As a result,after 20,000 miles of operation the temperature necessary to achieve 50-percent conversion of isopentane in a mixture of 0.2 percent isopentane, 2 percent carbon monoxide and 4 percent oxygen, and the balance nitrogen at 10,000 hourly space velocity has risen from 400° C. to 500° C. even with a catalyst taken from the exit portion of the catalyst bed. The rest of the catalyst was more severely affected. Therefore, it would appear that operation for 20,000 miles is near the limit for a catalyst.

Jan 1, 1963

By Edward W. Parsons

Conventional rock-bolt anchors often fail when installed in weak formations. The purpose of this work was to develop an anchor that would utilize an explosive charge to secure anchorage in any type of rock. Laboratory work to develop a rock-bolt anchored by explosive forming was initiated using rock-bolt models which had a drilled explosive chamber and were composed of various metals. This was followed by the use of several types of seamless tubing which were expanded with a water-coupled explosive capsule. By attaching a length of solid bolt to the anchor tube, a prototype explosive-anchored rock bolt was made. More than 150 laboratory models were expanded during this phase of development, During two field tests in underground mines (A and B) and one in an open- cut mine (C), 87 explosive-anchored bolts, 9 slot-and-wedge bolts, 2 bolts anchored with expanding grout, and 28 expansion-shell bolts consisting of three types of shells were installed and subjected to pull tests. The field tests were run to determine the effects of variables such as the amount and placement of the explosive charge, design changes in the bolt, and the effect on anchorage of different pull-test techniques. The field tests revealed the following: Mine A. The explosive-anchored rock bolt was feasible, but changes were necessary in bolt materials and in some details of bolt design. Mine B. The design and materials of the bolt gave excellent results in hard fractured rock, but no information was obtained concerning variations in the dimensions of the anchor unit or in the explosive charge. Nine C. Varying the explosive charge to produce a beaded surface on the bolt tube and tightening of the anchored bolt before pull-testing were found to increase significantly the anchorage obtained in soft ground.

Jan 1, 1963

By G. T. Krempasky

This report covers the installation and evaluation of lb reinforced concrete sets, 6 in each of 3 mines in the Goeur d'Alene mining district, Shoshone County, Idaho, and is the second of a series to determine the feasibility of a more permanent type of mine support. Closure measurements, where applicable, were made periodically of the concrete-set installations and were compared to the initial cross section of the sets. A different method of blocking was used at each test site; at one test site the type of blocking was changed several times during the test. Results from each test site are reported separately. No attempt was made to compare the cost of the concrete installations with the cost of other types of support used in the district. Such an evaluation of permanent types of support would require a longer period of time. At this time, tests are not complete enough to determine the applicability of underground concrete supports. However, results to date tend to confirm the general opinion that precast concrete mine supports could be used to advantage in openings that require support and must have long life, especially where decay of timber is an important factor.

Jan 1, 1963

By R. E. Mussier

This investigation was made to study new methods to prepare high-purity yttrium metal, Various methods were used to prepare pure intermediate compounds, primarily chlorides, bromides, and iodides, which were subsequently reduced to metal. The process found most suitable for the preparation of pure anhydrous yttrium chloride involved thermal dehydration of a mixture of hydrated yttrium chloride and ammonium chloride while under vacuum. Yttrium bromide and iodide were prepared most effectively by the direct halogenation of yttrim carbide. Yttrim carbide was obtained by reacting and melting yttrium oxide-carbon mixtures in a carbon-arc furnace. Yttrium halides were purified by vacuum distillation and reduced by alkali or alkaline-earth metals. Lithium and sodium proved to be the best reductants from the standpoint of yield (>95 pct) and purity (>99.8 pct) of the yttrium. The product of the reduction step was sponge metal, which was consolidated readily by conventional cold-mold, arc-melting procedure. The purest yttrium obtained in laboratory scale work was prepared by sodium reduction of yttrium chloride and contained only 125 pp oxygen; other impurities did not exceed 1,000 ppm. In larger scale tests yttrium containing only 800 to 1,000 ppm total impurities was obtained by lithium reduction of yttrium chloride. The tensile properties of high-purity yttrium were determined. Mechanical tests showed that yttrium can be forged, extruded, rolled, spot welded, and deep drawn.

Jan 1, 1963

By Wilbur I. Duvall

Twelve millisecond delayed blasts in four limestone quarries in Iowa were instrumented with arrays of vertical velocity gages to determine if the direction of propagation through the rock or the method of initiation of the blast had any effect upon the level of vibration. Two gage arrays approximately 90° apart were used to test the effect of direction of propagation. The vibrations from blasts initiated by three methods were recorded. Vibration records from these tests were analyzed for peak particle velocity as a function of distance from the blast. The data are shown to fit a power Law equation. Direction of propagation is shown to affect the value of the exponent n. The effect of charge size per delay interval on the level of vibration is removed from the data by scaling the travel distance by the square root of the charge weight per delay period. The method of initiating the blasts is shown to have a strong effect upon the level of vibration and the spread in the data from one shot to another.

Jan 1, 1963

By H. E. Powell

This study was made to determine the capabilities and limitations of the hydrocyclone for separating quartz sand from impure clays, Optimum operating conditions for beneficiating typical subgrade clays were determined. Estimates are furnished for installation and direct operating costs of hydrocyclones in such separations. Laboratory models of commercial hydrocyclones were used to beneficiate a suite of fire clays including plastic, semiflint, and flint types, all of which were contaminated with quartz in amounts ranging from 3 to more than 62 percent. Results show that this technique is not limited to a single type of clay but is applicable to clays ranging from plastic through flint, Under proper conditions use of this technique will result in good separation of the sand and good recovery of a useful clay mineral concentrate. Rejection of quartz from the clays investigated ranged from a low of 82.4 percent with an alumina recovery of 71.2 percent to a high of 99.0 percent with an alumina recovery of 85.6 percent.

Jan 1, 1963

By Thomas M. Nasiatka

Tests with a high-pressure water jet were conducted in the steeply pitching Roslyn No. 5 bituminous coalbed in the Roslyn No. 9 mine, Roslyn, Wash., to determine the feasibility of extracting coal from pillars and from a solid coal face in development without drilling and blasting. During pillar mining, using a hand-held monitor, the best results were obtained with a 0.150-inch- diameter nozzle, a water pressure of 3,500 psi, and a flow rate of 38.5 gpm.3 The rate of mining and productivity were 0.74 ton per minute and 16.6 tons per man-shift, respectively. During development mining, using a monitor mounted on a roof jack, the best results were obtained with a 0.148-inch-diameter nozzle, a water pressure of 4,500 psi, and a flow rate of 40.0 gpm. In one section of the mine where the coal was relatively hard, the rate .of mining and productivity were 0.10 ton per minute and 5.7 tons per man-shift, respectively in another section of the mine where the coal was relatively soft, the rate of mining and productivity were 0.51 ton per minute and 8.3 tons per man-shift, respectively. The tests showed that hydraulic mining methods were more productive than conventional mining methods in pillar mining. In development the productivity of hydraulic mining depended primarily upon the coal hardness. Compared with conventional methods, hydraulic mining methods were less productive where the coal was relatively hard and equally as productive where the coal was relatively soft.

Jan 1, 1963

By Martin H. Rogoff

The presence of antibiotic materials extractable with polar organic solvents was demonstrated in coals of various ranks. Since these antibiotics occur in low concentrations, 200 pounds of a high-volatile C coal was extracted with acetone at room temperature to obtain sufficient material for detailed study. The biologically active materials in the extract were concentrated by extracting with aqueous sodium hydroxide. The fractions soluble in sodium hydroxide inhibited bacterial cultures when present in concentrations comparable to those at which other antibiotics are active (5 µg/ml). Steam distillation of the extracts did not yield highly active materials, contrary to the finds of other investigators. Mass spectrometry of the extract indicated, mainly, the presence of 6-ring compounds in the region of mass 324 to 392. The predominance of 3-ring aromatic systems found by ultraviolet analysis suggests compounds such as biphenanthryl or similar structures. The activity of the hydroxide- soluble material decreased markedly when the phenolic hydroxyl groups were transformed into trimethylsilyl ethers. Hydrolysis of the ethers yielded a product having the same activity as the original material, which indicates that phenolic compounds are largely responsible for the antibiotic activity observed.

Jan 1, 1963

By R. V. Lundquist

The Bureau of Mines made a laboratory study of the amenability of anorthosite rock ( from the San Gabriel Mountains , Los Angeles County , Calif . ) to treatment by the lime soda sinter process for the extraction of alumina . The study was done under a cooperative agreement with the California Division of Mines and Geology . This report presents the results of the investigation , and it includes a review of the geology of the deposit ( 7 ) by Dr. Gordon B. Oakeshott . Interest in the recovery of alumina from submarginal aluminum silicate ores is stimulated by the fact that the domestic aluminum industry depends on imports of bauxite for its alumina requirements . Of the 8.0 million long dry tons of high - grade bauxite consumed in 1961 for producing metallurgicalgrade alumina , only 0.9 million long tons , or 11 percent , was mined in this country . During past years many organizations have carried out research programs to determine if alumina could be extracted economically from such domestic ores as clays ( 3 , 4 ) , anorthosite ( 8 ) , and other silicate sources . Successful alumina extraction is the ultimate objective of the Bureau of Mines program.

Jan 1, 1963

By Paul W. Johnson, Ralph C. Kirby, Frank A. Peters

An evaluation is presented for a process designed , on the basis of published work , to extract alumina as potassium alum from clay using sulfuric acid and potassium sulfate . The silica residue is separated by filtration . Ferric iron is reduced to ferrous iron , and the alum is crystallized from the solution , leaving the ferrous iron in solution . The alum crystals are separated from the solution and redissolved for feed to autoclave decomposition . In an autoclave the alum is partly decomposed to a basic alum , recovering five - ninths of the sulfuric acid and two - thirds of the potassium sulfate without using an acid plant . The basic alum is decomposed by calcining , and the potassium sulfate is then removed by washing with water . Operating costs for a plant producing 1,000 tons of alumina a day are estimated at $ 96.15 per ton of alumina . The fixed capital cost is estimated at $ 155 million . This process is not competitive under current economic conditions with the production of alumina from bauxite by the Bayer process . Improvement in leaching , basic alum decomposition , and washing could reduce the costs and improve the product which contains some potassium .

Jan 1, 1963

By T. E. Gray, A. W. Deurbrouck

This report describes the preparation characteristics of significant coalbeds in Kanawha County , W. Va . It is one in a series of Federal Bureau of Mines reports planned to determine coals suitable for producing metallurgical coke , either as mined or after beneficiation . Almost 9.4 million tons of coal was produced in Kanawha County , W. Va . , in 1959 , of which about 67 percent was cleaned mechanically in 10 cleaning plants . It has been estimated that more than 5,505 million tons remain in the county . Samples were collected from Pittsburgh , Stockton - Lewiston , Winifrede , Cedar Grove , Peerless , Upper Kittanning , Coalburg , Powellton , Eagle A , No. 2 Gas , and the Lower Kittanning beds . These beds were selected by the Bureau based on current production rates and estimated minable reserves . Float - and - sink tests of the samples collected from Eagle A , Peerless , Cedar Grove , Winifrede , and No. 2 Gas beds show that these coals at one location each are suitable for metallurgical use without washing . Lower Kittanning bed at four locations ; Pittsburgh , Stockton - Lewiston , and No. 2 Gas beds at two locations each ; and Coalburg , Powellton , Winifrede , Peerless , Upper Kittanning , and Cedar Grove beds at one location each can be upgraded to metallurgical quality by mechanical cleaning . Crushing the samples to 3/ 8- inch top size increased yields substantially at 1.30 specific gravity of Pittsburgh ( 17.5 percentage points ) and Upper Kittanning ( 13.0 percentage points ) beds and increased yield for the other beds sampled to a lesser amount . At this specific gravity , finer crushing caused In the 1.58 specific gravity float a general decrease in ash and sulfur . fractions of the other samples tested , most of the yields , and ash and sulfur contents , were lowered slightly by finer crushing .

Jan 1, 1963

By Albert W. Deurbrouck

This report describes preparation characteristics of significant coalbeds in Tazewell County , Va . In 1961 Tazewell County produced 933,110 tons of clean coal from six coalbeds ; the Lower Banner , Raven , Jawbone , Upper Seaboard , and Pocahontas No. 3 and No. 5. Samples from all of these beds , except the Lower Banner , were included in this study plus a sample from the Pocahontas No. 4 bed . Of the samples collected , only one would require upgrading to be of metallurgical quality . The coals ranged in rank from high- volatile -A to low- volatile bituminous .

Jan 1, 1963

By L. G. Trudell, J. W. Smith, K. E. Stanfield

Representation of actual oil yields from sections of the Green River formation oil shales by two types of drill - cutting samples was evaluated . Average oil yields of single sets of mud cuttings from hydraulic rotary drilling in Colorado and gas cuttings from pneumatic rotary drilling in Utah were compared statistically with yields of core samples taken from adjacent holes . Oil yields from gas cuttings were identical to oil yields of core samples . Mud cuttings appeared to represent a section of the formation conservatively , the deficiencies increasing with increasing richness of sample . Because a large amount of the oil - yield data currently available for the Green River formation is based on mud- cutting samples , development of a valid correction method by additional testing is needed .

Jan 1, 1963

By T. E. Green, E. F. Spano, W. J. Campbell

A combined ion - exchange X- ray spectrographic method was developed and evaluated for determining trace amounts of cobalt and nickel in high - purity tungsten and tungsten trioxide . The sensitivity for both cobalt and nickel is in the range from 0.2 to 0.5 μg ( 0.04 to 0.1 ppm , based on 5 gram samples ) . Accuracy at the 5 to 20 μg level is ±10 percent of the amount present . Approximately 16 hours elapsed time is required for analysis

Jan 1, 1963

By Michael G. Zabetakis, Aldo L. Furno, Henry E. Perlee

The Bureau of Mines conducted an experimental study with liquid and gaseous hydrogen to determine the hazards associated with the use of liquid hydrogen as an ionizing particle detector in bubble chambers . The glass window , the vacuum chamber , and the vent system were investigated . In addition , a study was made of the detection and ignition of escaping hydrogen and of the available electrical equipment for use in hydrogen atmospheres . Materials such as tempered glass , aluminum , and stainless steel are not penetrated readily by the small fragments formed when fully tempered glass is shattered and propelled by hydrogen at initial pressures up to 100 psig ; long , slender fragments from untempered glass may penetrate thin walls of relatively soft materials such as rubber gaskets and lead . Hydrogen can be vented satisfactorily from a vacuum chamber with a well - designed vent system . However , the rapid leakage of hydrogen into the surrounding air is a serious problem because the available detectors are satisfactory only when the accumulation of hydrogen is slow . Much of the electrical equipment currently available was designed for use in hydrogen- air atmospheres .

Jan 1, 1963

By H. P. Hamlin, W. A. Grosh

Samples of clays , shales , and argillites from 21 locations were subjected to preliminary bench- scale tests for bloating properties , and several samples were tested for ceramic properties . Samples showing favorable bloating properties were further tested in a pilot - plant - scale rotary kiln . Physical characteristics and concrete -making properties of the bloated products were determined . The Decorah shale from one area made a suitable material for a lightweight aggregate ; however , the limestone layers in the formation must be eliminated or the resulting activated lime must be controlled by quenching .

Jan 1, 1963

By R. H. Storch, D. C. Holt

During reconnaissance investigations of more than 300 stream areas in Idaho to determine the potential value of ilmenite in black - sand placer deposits 46 deposits were explored by churn drilling , trenching , test pitting , or shafting . The component mineral content and total black - sand content were determined for more than 8,690 reconnaissance and exploration samples . Data compiled during the investigation indicate a good potential for large , low- grade deposits containing ilmenite , monazite , columbite , euxenite , uranothorite , and other radioactive black minerals and accessory black - sand minerals . The data also indicate most deposits will be economic only if several component minerals can be recovered as coproducts .

Jan 1, 1963