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By Nancy S. Raymon

The Bureau of Mines investigated the effect of controlled additions of selected metal oxides, as well as the adjustment of the calcia-to-silica ratio on the high-temperature strength of refractory-grade periclase. Increases in the hot flexural strength of some periclase materials in the range of threefold to fourfold were obtained with additions of Zr02 and by adjustment of the CaO:Si02 ratio to the 2.5 to 3.0 level. Results show that for each periclase refractory raw material, there exists a combination of level of Zr02 addition and an adjustment to the CaO:Si02 ratio that optimizes the hot flexural strength of each of these materials. Data also indicate that the improved hot strengths can be attributed to the high-temperature secondary phases formed between the different levels of periclase impurities and the additives, resulting in improved intergranular high-temperature bond strength.

Jan 1, 1982

By K. P. V. Lei

The Bureau of Mines as part of its research effort to minimize the generation of hydrometallurgical waste, investigated a sodium sulfide leaching-electrolysis procedure for treating hydrometallurgical residues for elemental sulfur and base-metals recovery. Research was conducted on a leaching residue from a lead concentrate. The following procedure was developed. 1. The elemental sulfur was dissolved as polysulfide with an Na2S solution. 2. The resultant metal sulfide bearing residue was oxidatively acid leached in a cationic membrane electrolysis cell; the metals were solu¬bilized at the anode, and a base was generated at the cathode. 3. The elemental sulfur was recovered from the polysulfide solution by neutralizing with the acid in the anolyte. Byproducts of the neutralization were H2S and a sodium salt solution. 4. Sodium sulfide was regenerated by reacting the H2S byproduct with the base in the catholyte. 5. Lead as PbCL2 was recovered from the anode residue by brine leaching, and the other metals were recovered from the sodium salt solution as metal sulfides. 6. The barren filtrate from the metal sulfide precipitation constituted the recycled electrolyte. Ninety-eight percent of the elemental sulfur, 98 pct of the lead, and up to 80 pct of other accessory metals were recovered from a residue obtained from the FeCl3-NaCl leaching of a lead concentrate.

Jan 1, 1982

By R. H. Lien

The Bureau of Mines has conducted research on a flue gas desulfurization (FGD) process as part of its goal of minimizing the undesirable environmental impacts associated with sulfur dioxide (S02)-bearing waste gases. This FGD process, referred to as the modified citrate process, involves absorption of S02 in a buffered citric acid solution. The absorbed S02 is subsequently stripped from the solution using steam, which regenerates the solution and produces a wet S02 product. This product can be further processed to make sulfuric acid or liquid S02. Economic evaluations showed the process to be expensive when the stripper was operated at or near ambient pressures because of the large amounts of steam required for solution regeneration. Research was directed at reducing steam consumption in the stripper. The effect of stripper pressure on steam consumption was investigated. A process research unit (PRU) was operated with the stripper pressurized in the range of 5 to 150 psig. Test results showed that steam consumption decreased with increased stripper pressure. For example, when operating the PRU stripper at 150 psig, 4.1 grams of steam per gram of S02 was required to remove 90 pct of the S02 from a 1.0-vol-pct-S02 gas. This compares to 7.1 grams of steam per gram of S02 required for 90-pct S02 recovery at 5 psig.

Jan 1, 1982

By Robert J. Timko, Edward D. Thimons

Sulfur hexafluoride (SF6) is an odorless, colorless, nontoxic gas that has found acceptance as a tracer gas in research on ventilation pat- terns, measurement of air leak rates, respirable dust reductions due to bagging hood modifications, and the study of airflows relating to gob boreholes. Following a short review of the SF6 sampling technique, this report describes recent Bureau of Mines projects in which SF6 was used successfully as a tracer gas, enabling researchers to acquire representative data quickly and inexpensively.

Jan 1, 1982

By Theodore L. Turner

This Bureau of Mines report describes calcination of kaolinitic clay in a direct-fired 2-1/2- by 24-ft rotary kiln at 750° and 775° C. Methods for preparing kaolin feed materials and characterization of calcined products are discussed. Approximately 99 pct of the alumina in a typical eastern Georgia kaolin was soluble in HC1 after calcination at either 750° or 775° C.

Jan 1, 1982

By J. I. Paige

The Bureau of Mines studied methods for recovering unreacted titanium minerals and petroleum coke from titanium chlorination plant wastes prior to neutralization treatment with lime. The objective was to recover valuable raw materials and to reduce the amount of waste materials that must be treated for disposal. Samples of solid wastes were physically beneficiated by gravity concentration (tabling) to recover titanium minerals containing 69.0 to 92.4 wt-pct Ti02 and by selective carbon flotation to recover petroleum coke containing 94.0 to 96.8 wt-pct C. Laboratory data indicate that the recovered titanium mineral would decrease the amount of solid waste to be disposed of from 32.8 to 53.9 wt-pct. The recovery of coke would further decrease the amount by additional 32.9 wt-pct. Preliminary tests conducted on recovering vanadium, chromium, and columbium from liquors obtained by leaching chlorination residues also have shown that (1) 97 pct of the vanadium was extracted from leach liquors in a two-stage solvent ex-traction procedure and (2) 58 pct of the columbium and 40 pct of the chromium were separated from the leach liquors by an ion exchange technique using a strong acid resin.

Jan 1, 1982

By Connie S. Musulin

The Bureau of Mines conducted an experiment at Exxon Mineral Co.'s Buffalo Shaft Operation to determine the time required for radon concentrations to return to a base average after fan shutdowns. Shutdown times ranging from 5 min to 16 hr were evaluated. An equation was derived to calculate a ratio that determines the time required for the radon concentration to return to the average level that existed in the mine prior to shutdown. For fan shutdowns of 15 min or more, underground personnel should be evacuated to areas with natural downcast ventilation. For shutdowns of less than 1 hr, personnel should not return to the working area until the elapsed time is four times the shutdown, or until the working area is resampled and found safe. If the mine is not in production during weekends, the downcast fans can be turned off .from midnight Friday until 4 p.m. Sunday, and the radon daughter concentration should be below 1 WL throughout the mine by the start of the shift Monday. This fan shutdown would conserve energy and save the mining company an estimated $21,000 each year.

Jan 1, 1982

By L. W. Brandt

As part of its objective to expand the body of mineral information as a basis for new technology, the Bureau of Mines conducted research on the fundamental behavior exhibited by phosphate clay waste in settling ponds. A semiempirical equation used to describe the compaction of ceramic powders in a single-acting die was applied to aqueous phosphatic clay waste and attapulgite slurries. This equation, [*V = a1 e ?k1/P + a2e ? k2/P] was found to describe the compaction of an attapulgite gel and a phosphate slime gel by a moving screen. [*V] is the ratio of the compaction achieved at a given pressure, P, to the compaction achieved at a pres-sure sufficient to remove all space between particles. The constant al represents the fraction of compaction achieved at low pressure by rearrangement of floes to higher packing density, and a2 represents the fraction of compaction achieved at higher pressure resulting from removal of voids within floes. K1 and K2 are constants determined from the experimental data. Both the low-pressure and high-pressure compaction mechanisms were observed in the compaction of the clays. These two compaction mechanisms offer an explanation for the observation that impounded slimes initially dewater rapidly and then dewater at a much slower rate.

Jan 1, 1982

By John A. Breslin

The Bureau of Mines measured respirable dust in coal mines by means of multiple dust samplers worn by persons moving about the mines. The measurements were made primarily to evaluate the effectiveness of certain dust-control techniques; however, for this report, the data have been analyzed to determine the precision of the personal dust-sampling measurements. A total of 68 sets of measurements were available from multiple personal samplers. The measured dust masses were less than 1.0 mg because the sampling times were short. The coefficient of variation calculated from these data was 18.5 pct, compared with coefficients of variation ranging from about 10 to 30 pct, which were calculated from the most precise and extensive data available for fixed-point dust measurements made in coal mines. From this comparison, it is concluded that dust samplers worn by personnel are as precise as fixed-point samplers in measuring respirabe coal dust; the wearing of the samplers by someone moving about a mine does not contribute significantly to the variation in measurements made with these instruments.

Jan 1, 1983

By Annie G. Smelley

As part of its program to develop technology that will encourage maximum utilization of the Nation's mineral resources, the Bureau of Mines conducted research on debrining potash-clay waste slurries by means of flocculation with a high-molecular-weight polymer and subsequent solid-liquid separation on a rotating trommel screen. In laboratory batch tests, potash-clay waste slurries were consolidated from initial clay contents of 8 pct to final contents of 30 pct with a polymer dosage of 1.2 Ib/ton of dry clay waste. Small-scale continuous tests yielded debrined products containing 20 pct solids using a polymer dosage of 1 Ib/ton of dry clay solids.

Jan 1, 1983

By D. C. Fleck

The Bureau of Mines, in a cooperative research program with four lead companies, has investigated ferric chloride leaching of galena to prepare lead chloride for molten-salt electrowinning to produce lead metal. The hydrometallurgical-electrolytic process is an alternative to the sintering-smelting-refining process currently used to produce lead metal and avoids the environmental problems associated with a conventional smelter. During investigations on the electrowinning aspects of the work, it was noted that certain cations, moisture, and sulfate in the electrolyte affect lead metal purity, cell voltage, current efficiency, and viscosity of the electrolyte. Results of bench-scale tests are re-ported on the effects of CaCI2, CuCI2, FeCI2, MgCI2, NaCI, ZnCI2, PbS04, and moisture on electrolysis. As impurities increased in the electrolyte, current efficiency decreased. CaCI2, CuCI2, and FeC12 decreased current efficiency by 12 to 47 pct. ZnCl2 gave a small voltage increase, while CaCI2 addition equivalent to 4.9 pct Ca caused a 50-pet increase in voltage. The lead metal was contaminated in direct proportion to the CuCI2 buildup in the electrolyte, Anode corrosion was observed with MgCI2 and MgC12?6H20. Viscosity increased appreciably with the buildup of NaCI, CaCI2, and sulfate. Electrolyte foaming occurred with ZnC12, MgC12?6H20, MgC12, FeC12?2H20, and FeCI2. Moisture inhibited the coalescence of the lead metal.

Jan 1, 1983

By Roy C. Bartholomae

This Bureau of Mines report presents the results of a laboratory investigation of coal cutting mechanics and noise. These experiments were performed using linear cutting apparatus that operates over a broad cutting speed range. The influence of several coal cutting parameters on the noise, force, productivity, and specific energy associated with linear cuts was ascertained. Some basic theoretical aspects of coal cutting mechanics and noise generation are discussed, and the results of the laboratory experiments are used to formulate analytical models of the coal cutting forces and noise. The analytical model for coal cutting noise is then generalized to account for the more important effects of rotary cutting. Based on the generalized model, an estimate of the sound pressure level at an operator's position is made for a typical continuous mining machine. It is concluded that by employing linear rather than rotary cuts, using deeper depths of cut, slower cutting speeds, and more efficient cutting tools, it is possible to reduce the level of coal cutting noise, as well as provide benefits to other important areas of health and safety in underground mining.

Jan 1, 1983

By R. S. Olsen

The Bureau of Mines is engaged in research to recover aluminum from kaolinitic clay and other nonbauxitic domestic resources. As part of this work, calcined Georgia kaolin was prepared by a process that prevents slime formation and makes the leached residues fast settling and easy to filter. The leaching reaction for calcined kaolinitic clay in a 5 pct stoichiometric excess of boiling 23-to 26-pct HCI was found to be zero order. Rate constants based on the weight-fraction of aluminum in the clay were found to be between 0.095 and 0.15 min-1 depending on feed preparation and leaching parameters. The mathematical relationships between aluminum extraction and time for both batch and continuous, stirred-tank operations were derived and verified experimentally.

Jan 1, 1983

By M. J. Ferrante

The Bureau of Mines determined the enthalpies of Ni3S2 relative to 298.15 K to provide new thermodynamic data for advancement of mineral science and technology. Enthalpies were measured with a copper-block calorimeter from 298.15 to 1,197 K. A solid-solid transition was found at 834±1 K, with an isothermal heat absorption of 13.32 kcal/mol. The temperature of this solid-solid transition was accurately measured by differential scanning calorimetry. Because Ni3S2 does not melt congruently, the heat of fusion of 4.70 kcal/mol was obtained by extrapolation of enthalpy measurements from the solid and liquid phases to approximately 1,064 K. Tabulated values are given for the relative standard enthalpy, heat capacity, entropy, and Gibbs energy function between 298.15 and 1,800 K. Enthalpies are also given in equation form and combined with data from the literature to derive values of standard enthalpies of formation and Gibbs energies of formation. Similar calculations were made for the reaction of crystalline and liquid nickel with gaseous diatomic sulfur for Ni3S-2(c, l).

Jan 1, 1982

By Roy E. Peterson

The Bureau of Mines conducted bench-scale research to evaluate materials which showed potential as low-cost reductants for use in the ironmaking industry. These materials were lignite, subbituminous coal, coal char, tree trimmings, refuse--derived paperboard, used crankcase oil, and peat. To compare their effectiveness, the materials were tested in the reduction roasting of nonmagnetic taconite and, except for oil and peat, in the reduction of iron oxide pellets to metallized pellets. Reduction was conducted in a 18-cm-diameter, rotary drum, which was externally heated in an electric furnace. Over 92 pct of the iron was magnetically recovered from a nonmagnetic taconite after roasting with any of the reductants, but greater quantities of reductant were required to achieve this when the waste materials were used. The fossil fuels were also more effective for metallizing pellets, although metallizations above 90 pct were also obtained with tree trimmings and refuse paperboard. However, refuse paperboard had to be frequently recharged to the furnace because it depleted rapidly.

Jan 1, 1983

By Sam G. Demou

Drag bit cutting tests were conducted chiefly to determine bit forces encountered in rock types representing a range of compressive strength and hardness and thus enable the design engineer to estimate a continuous miner's performance in a range of rock types. Testing was carried out on the Bureau of Mines uniquely designed, instrumented rock cutting device (RCD). This device can make 3-ft-long cuts at various depths and speeds to approximate full-scale drag bit cutting by continuous miners. Point attack and cutter bits were tested on four rock types ranging in compressive strength from 7,200 psi (trona) to 29,600 psi (Valders white rock). Cutting tests were made at depths up to 1 in and speeds up to 70 in/sec. Data included normal and cutting forces, groove depth, groove width, and weight of rock broken. The effect of varying the cutting speed was determined, and specific energies were calculated for the various conditions. The bit wear was also observed. For the rocks tested, compressive strength and hardness are good indicators of forces, specific energy, and wear encountered. Results, especially bit wear observations, show the possibility of extending continuous miners, already being used in trona, to Indiana limestone (10,000 psi). Rapid bit deterioration precludes use in Tennessee marble (16,800 psi) and Valders white rock (29,600 psi).

Jan 1, 1983

By G. R. Smith

Critical and strategic metals are often present in small quantities in low-grade domestic ores. When these ores are leached, the resulting solution usually contains the metals in very dilute quantities. Selective electrowinning from dilute electrolytes was investigated by the Bureau of Mines. A metal deposit containing 84 pct nickel was electrowon from the leach solution of a complex domestic ore bulk flotation concentrate originally containing approximately 2 wt-pct nickel. Key to achieving accelerated deposition rates, in the case of dilute solutions, is the rapid movement of the electrolyte through the electrowinning cell. Pure, synthetic nickel electrolytes were used to establish deposition parameters, and to optimize electrolyte velocity or mass transfer rates. Hydrodynamic and electrodeposition parameters for both the synthetic and leach electrolytes are presented and the experimental research described. Selective electrowinning appears to offer a viable alternative to physical separation methods to obtain separate metal "concentrates" from low-grade ores.

Jan 1, 1983

By H. C. Ko

The Bureau of Mines maintains an active program in thermochemistry to provide thermodynamic data for the advancement of mineral science and technology. As part of this effort, the standard enthalpy of formation at 298.15 K, ?Hf°, for 2CdO-CdSO4 was determined by HCI acid solution calorimetry to be -345.69 ±0.61 kcal/mol.

Jan 1, 1983

By I. D. Shah

The copper-nickel ore of the Duluth Gabbro Complex in northeastern Minnesota is a large potential domestic resource of cobalt and platinum-group metals. However, because of the low grade of the primary metal values (0.5 pct Cu, 0.15 pct Ni), the private sector has assigned a relatively low priority to the development of technology for processing this ore, anticipating that mining probably would not begin until the mid-1990's. Furthermore, preliminary processing flowsheets considered by the mining companies centered on the primary metal values. As part of an effort to help provide the basis for technology to recover critical and strategic minerals from domestic resources the Bureau of Mines is investigating methods to recover all of the mineral values, in the Duluth Gabbro material, with particular attention to the byproduct critical minerals. A key step in this process is the removal of a relatively large amount of iron present in the bulk sulfide flotation concentrate to permit subsequent extraction of mineral values. This report describes a direct smelting method that removes most of the iron and produces a copper-nickel-cobalt matte, an intermediate product from which the metal values subsequently are separated. Copper, nickel, and cobalt grade and recovery data are presented for the direct smelting method. Test results showed that under certain conditions some of the mineral values reported to the slag, requiring slag cleaning to recover them.

Jan 1, 1983

By Elizabeth A. Johnson

The effect of slag composition on lead losses to slags and on the behavior of associated accessory elements in lead blast furnace smelting has been studied by the Bureau of Mines. Equilibrations of 30 g of lead and synthetic slag doped with Cu, In, TI, and Sb at 1,200° C in CO-C02 atmospheres revealed the importance of the FeO:Si02 ratio and the basicity ratio, (CaO+MgO):SiO2, of the slag. Lead losses to slags increased with an increasing FeO:Si02 ratio and decreased with an in-creasing basicity ratio. Copper and indium distribution coefficients, [Lx =] increased from 15 at the lower basicity ratios to near 60 at higher basicity ratios. LTI values increased from 20 to 150 as slag basicity increased. Lcu, Lin, and LTI were relatively in-dependent of the FeO:Si02 ratio, but increased with greater amounts of accessory elements in the system. Antimony distribution alone was shown to be strongly affected by FeO:Si02 ratio, although data were scattered. LSb values ranged from 20 to 800 and decreased sharply with increasing FeO:Si02 ratios. The basicity ratio and the level of accessory element load did not have any noticeable effect on LSb.

Jan 1, 1983