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By R. J. Gajan

As part of its research program on secondary metal refining, the Federal Bureau of Mines has developed a fast method for determining aluminum, iron, copper, cadmium, and lead in zinc-base alloys. The new method is intended for use by trained technicians in laboratories with inexpensive equipment. It can be used either in the analytical laboratories of the many small plants that are characteristic of the secondary metals industry or in laboratories engaged in basic research to improve refining processes. A complete analysis for the foregoing elements can be made in less than 3 hours from a single sample in solution. The method is especially helpful when a small amount of sample is available. Aluminum and iron are determined spectrophotometrically and the other elements polarographically. The new method is now being used for control analysis in metallurgical research, and the results compare favorably with previously used spectrographic methods. Luke and Braun4/ described a photometric method for the determination of aluminum in zinc diecasting alloys in which the aluminum was complexed with Aluminon reagent (ammonium salt of aurintricarboxylic acid), forming a red lake. An adaptation of this method was used for determining aluminum. Beers law is obeyed between 0.01 and 0.06 milligram of aluminum.

Jan 1, 1961

By Robert H. Raring

Viewed abstractly, a mill may be defined as a mineral processing facility located somewhere between the mine and the tailings storage area, Just how mining operations and the demands of tailings storage affect mill design is, the subject of this paper. At the outset, it will be readily acknowledged that no two installations can, or ever will be the same. At one extreme is the bucket line dredge where the distance between the ?mine? and the tailings area is measured in terms of tens of feet. At the other extreme, the large open pit copper mines are frequently spread across twenty, miles or so of countryside with the ore moving to the mill, as exemplified by the operations at Bingham Canyon, Ray, or Ruth - the "upstream" counterparts of Garfield, Hayden and McGill. In each of these cases, mill location was largely determined by requirements for tailings storage and/or water supply.

Jan 1, 1961

By Samuel P. Polack

This report reviews investigations to determine the fire hazard in coal mining when using flammable petroleum hydraulic oils to actuate mining equipment and summarizes research by the Bureau of Mines and industry on fire-resistant hydraulic fluids. Tests were established to evaluate fire resistance and the necessary characteristics to assure adequate service when fire-resistant fluids are used to replace petroleum hydraulic oils. The research was conducted in the laboratory and field trials under actual operating conditions in underground mines. Bureau of Mines Schedule 30 became effective December 17, 1959; the first approval was granted on February 18, 1960, and the twelfth was granted on March 17, 1961. The approvals include nine ready-mixed (by the producer) fluids and seven concentrates to which water is added by the user according to instructions from the producer. Seven synthetic-type fire-resistant hydraulic fluids submitted by two producers are also approved. Over 100 coal mines are now using water-in-oil emulsion-type fire-resistant hydraulic fluids in varying degrees from a trial in one machine to all the hydraulic equipment in an entire mine.

Jan 1, 1961

By G. V. Jere, C. C. Patel

Chlorination of the various constituents of ilmenite by different chlorinating agents in presence of various reducing agents, have been considered on the basis of the standard free energy and standard enthalpy changes as a function of temperature. The standard free energy change considerations show that it is beneficial to chlorinate ilmenite by chlorine in the presence of carbon and also that iron constituent of ilmenite can be preferentially chlorinated by clzlorine, titanium tetrachloride or their mixture. These findilzgs have been corroborated from the published work. METALLURGICAL processes involving the use of titanium tetrachloride have gained in importance because of the use of the latter in the manufacture of titanium metal. Since ilmenite is more abundant in nature than any other titanium mineral, the future of the metallurgical processes depends on the utilization of ilmenite for the production of titanium tetrachloride. In these laboratories, investigations have been carried out on the chlorination of ilmenite under a variety of conditions.1'2 During these studies, it was noticed that 1) preferential chlorination of iron was effected at low temperatures (400° to 600°C) and at low carbon content (6 to 7 pct), 2) carbonyl chloride retarded the chlorination of iron oxides and titania perceptibly, while 3) carbon-tetrachloride, compounds of sulphur and some other catalysts favored the chlorination. Moles3 has found that oxides of iron are chlorinated in preference to titania at high temperatures, while wilcox4 has claimed the preferential chlorination of titania between 1200" and 1500°C. It has been shown in this paper that preferential chlorination of titania claimed by Wilcox is not likely to occur. Daubenspeck and coworkers5,6 have claimed the preferential chlorination of iron by chlorine or by a mixture of titanium tetrachloride and chlorine between 700° and 1050°C in the absence of carbon. Even when plain titanium tetrachloride is employed as the chlorinating agent, pascaud7 noticed the preferential chlorination of iron and other oxides. The purpose of this paper is to explain from thermodynamical considerations, the various chlorination reactions studied so far. ILMENITE CONSTITUENTS AND THEIR CHLORINATION PRODUCTS Although the general composition of the ilmenite mineral is represented as FeTiO,, most of the ilmenites found in nature have variable quantities of TiO2 (44.6 to 64 pct), FeO (4.7 to 36 pct) and Fe2O3 (6.9 to 28 pct).8 The higher content of ferric iron in ilmenites was attributed by Millerg to the presence of arizonite (Fe2O3.3TiO2). But the X-ray studies by Overholt, Vaw, and odd" have shown that arizonite is a mixture of haematite, ilmenite, anatase, and rutile. Except for the anatase, similar views have been advanced by Lynd, Sigurdson, North, and Anderson8 from magnetic, X-ray, and optical and electron microscope studies. The ilmenite ores can, therefore, be assumed to consist of mineral aggregates of ilmenite, rutile and haematite. From the free energy of formation of ilmenite (FeTiO3), it has been shown by Kelley, Todd, and King11 that ilmenite is stable even up to its melting point (1367°C) and would not undergo decomposition into its constituent oxides. Schomate, Naylor, and Boericke12 have found that in the presence of a reducing agent the iron constituent of ilmenite is selectively reduced. The reaction of chlorine with ilmenite in presence of a reducing agent can, therefore, be synonymous with that of the reaction of chlorine with the constituents of ilmenite, viz., TiO2, FeO, and Fe2O3. Most of the reaction products of chlorination of ilmenite in the presence of reducing agents will be in equilibrium with their dissociation products, depending on the temperature. The titanium tetrachloride is, however, quite stable up to 1500°C due to its covalent nature. The equilibrium for the ferric chloride system has been investigated by Kangro and Bernstorff, 13, schafer14 and Kangro and petersen,15 and the results are summarized in Fig. 1, curves a, b, and c respectively. From these results, it is clear that the ferric chloride disociates as follows: 324° to 700°C FeaCl6(g) ?2FeCl2(c) + Cl2(g) [1] 324°to 900°C Fe2Cl6(g) =2 Fe Cl2 Reaction [I] (curve a) occurs in the forward direction to about 6 pct at 400°C but falls off very rapidly with increase in temperature and beyond 600°C, it is practically negligible, perhaps due to the formation of the stable monomer, FeC13(g). As the temperature is further increased, the amount of FeCl,(g) in-

Jan 1, 1961

By J. E. Gray

Before specifications are discussed it may be well to define the term "Mineral Aggregates." Professor K. B. Woods (1) defined "Mineral Aggregate--An aggregation of sand, gravel, crushed stone, slag, or other material of mineral composition used in combination with a binding medium to form bituminous and portland cement concrete, macadam, mastic, mortar, plaster, etc., or alone as in railroad ballast, filter beds, and various manufacturing processes, such as fluxing, etc. " This definition is too all inclusive for the purposes of this paper; therefore, this discussion will be confined to specifications for natural aggregates which means sand and gravel and crushed stone, and limited primarily to coarse aggregate which is aggregate larger than one-quarter inch in size. To the uninitiated, this may seem to be a very limited subject on an unimportant material. However, aggregates are essential in all types of construction. The tonnage and value of these two aggregates produced in the United States during 1959 as reported by the Bureau of Mines were as follows: Sand and Gravel 729,895,000 tons valued at $728,527,000 Crushed stone 581,721,000 tons valued at $824,411,000

Jan 1, 1961

By P. K. Guerrero, N. Arbiter

The correlation of power consumed by a tumbling mill with the dimensions, speed, and load has been attempted by three principal methods. One of these, the torque formula, has been reviewed critically elsewhere.' This approach, while analytical, disregards the individual motion and speed of the tumbling bodies and assumes that the gross geometry of the entire load is sufficient to establish the power requirement. A more general approach, using dimensional analysis, has been applied in this laboratory by the present authors1'1, and more recently by Rose.3 This disregards the internal conditions within the mill entirely and in effect is an empirical procedure for correlating data. Finally, the complete analysis of tumbling mill dynamics as first made by Davis' attempts to develop the power requirement from individual ball and rod paths and velocities. Although Davis' result is applicable only at a single speed for a given size and load it could be useful, since his optimum speed is at the upper limits of conventional tumbling mill practice. Where power values predicted by the Davis equation were compared with actual mill requirements, they were found too low for small mills and much too high for the largest mills. This suggested that the agreement with actual intermediate range requirements might be fortuitous, and the development of the equation was examined critically. The probable source of error was found to lie in an erroneous assumption made by Davis in converting the energy of ball or rod motion to power. With the same approach, but with different assumptions, a modified equation has been obtained which predicts results that are usually consistently high. This is to be expected, since it is assumed that there is no slip between load and shell and no interference among tumbling bodies. Both these effects should account for the difference. Development of Equation: When a cylindrical shell charged with a substantial weight of rods or balls is slowly rotated about a horizontal axis, the load surface first assumes an inclination that gradually increases to a maximum. Continued rotation results in failure within the load, characterized by a sliding of the top layers down the slope and a reduction in the angle of inclination. Further rotation again increases the angle, and the cycle repeats. If the speed is increased, there is continuous load failure and build-up and a continuous stream of rods or balls descends over the upcoming mass, which moves in circular arcs. At higher speeds the up-

Jan 1, 1961

By J. R. Nettle

The purpose of these studies by the Federal Bureau of Mines was to determine the feasibility of refining low-grade hafnium by an inert-gas-shielded molten-salt electrorefining technique to produce a hafnium metal meeting reactor specifications. The techniques were adapted from those used success-fully for titanium electrorefining. Three electrolytes containing hafnium chlorides were developed from which deposits having a Brinell hardness of 170 or below were recovered. A KC1 + NaC1 + HfC14 electrolyte produced deposits in the hardness range of 140 to 165 Brinell. Deposits with a hardness range of from 132 to 152 Brinell were pro-duced from an electrolyte composed of KC1 + LiC1 + HfC14. A third electrolyte composed of NaC1 + K3HfC17 produced deposits with a hardness as low as 139 Brinell. In a fourth electrolyte, composed of NaC1 + K2HfF6, a measure of refining was accomplished, but under the test conditions no metal meeting specifications was recovered; none was softer than 174 Brinell. A number of metallic impurities were reduced in quantity by the electro-refining process, notably iron, which normally was reduced from 250 p.p.m. to less than 50 p.p.m. Magnesium generally was reduced from 680 p.p.m. to less than 80 p.p.m. Manganese content was also reduced by the electrorefining process. Sponge containing 90 p.p.m. Mn yielded deposits containing a maximum of 50 p.p.m.; some deposits contained only 10 p.p.m.

Jan 1, 1961

By E. G. King

Many of the existing thermodynamic values for the titanium halides are estimates, including all the entropies and high-temperature heat contents of their crystalline and liquid phases. This report contains the results of low-temperature heat capacity measurents (which lead to entropy values at 298.15° K,) and high-temperature heat-content measurements of four halides - trichloride, tribromide, tetrabromide, and tetraiodide. The new data are combined with selected heat-of-formation values at 298.15° K. to obtain improved values of the heats and free energies of formation of these halides at high temperatures, thus supplementing the previous data of Kelley and Mah.5/ ACKNOWLEDGEMENTS This investigation was conducted under a cooperative arrangement between the Federal Bureau of Mines and the Department of the Navy, Office of Naval Research. The work was done by Bureau of Mines personnel using Bureau of Mines calorimetric equipment. The Office-of Naval Research supplied the supporting funds and arranged for procuring the samples of the titanium halides. The samples were prepared and analyzed by the Inorganic Chemistry Section, Division of Chemistry, National Bureau of Standards.

Jan 1, 1961

By Dale W. Richardson

Ductile hafnium was not obtained consistently by the conventional Kroll process. The bimetal reduction modification produced a more ductile hafnium by lowering the impurities, especially oxygen, in the sponge metal. Hafnium oxide was chlorinated in the presence of carbon to form anhydrous hafnium tetrachloride, which was reduced by sodium and magnesium in an inert atmosphere to produce sponge hafnium metal. After vacuum distillation to remove the byproducts, the sponge was arc-melted into ingot and rolled into strip. Metallic impurities were decreased by evaporating the hafnium tetrachloride from a fused salt. An excessive amount (over 1,200 parts per million (p.p.m.)) of aluminum was contained in some of the hafnium oxide, much of which remained as aluminum chloride in the hafnium tetrachloride during chlorination. Evaporation of the hafnium tetrachloride from a fused NaCI-KCI mixture during the Mg-Na reduction greatly lowered its aluminum content, as most of the aluminum and some of the other metallic impurities were retained by the fused salt.

Jan 1, 1961

By M. J. Saarivirta, P. P. Taubenbla

This paper presents some high-temperature properties of copper-zirconium conductor alloy compared to copper-chromium alloy. Definite superiority of the copper -zirconium alloy over the copper-chromium alloy at high temperatures is shown. RECENT investigations have shown that cold-worked copper-zirconium alloy possesses good room-temperature strength, ductility, and conductivity and maintains most of its strength at temperatures up to 450°C (840°F). As a result, this alloy is now used for many applications, such as commutator segments, resistant welding wheels and tips, rectifier bases, electrical contacts, and so forth. Early investigations1-3 have shown that the maximum solid solubility of zirconium in copper is close to 0.15 pct and the alloy containing Cu-0.10-0.15 pct Zr exhibits the optimum mechanical and physical properties. Results2 have also shown that the alloy has better elevated temperature strength and ductility than copper-chromium and copper-silver alloys. The present investigation was undertaken to learn more about the elevated temperature properties of copper-zirconium alloy and to compare these properties with those of the copper-chromium alloy. WORK PROCEDURE The commercial copper-zirconium alloy, Amzirc was selected for this investigation. Because this alloy is composed of oxygen-free high-conductivity copper and 0.10-0.15 pct Zr, it was believed that possible disturbance from impurities would thus be negligible. Copper-chromium alloys used in this investigation contained 0.40 and 0.70 pct Cr and balance copper. The Cu-0.40 pct Cr alloy was a commercial brand, whereas the Cu-0.70 pct Cr alloy was made from OFHC copper and Cu-5 pct Cr master alloy. It was made in a graphite crucible under argon gas cover and cast. In the preparation of specimens, all three alloys were treated to give the optimum properties; thus the Cu-0.15 pct Zr alloy was solution annealed at different temperatures to determine the desirable solution annealing temperature. It was then cold worked and aged at 375" to 400°C (705" to 750" F). A solution annealing temperature of 1000°C (1830°F) was selected for the copper-chromium alloys because this temperature is widely used in commercial practice. The same alloy was aged at 450°C (840°F) after solution annealing and cold working. It was found that the maximum precipitation hardening of the copper-chromium alloy occurred at this temperature. When aged after solution annealing, the aging temperature was 500°C (930"F) for both alloys. The following properties were determined: 1) Tensile properties as a function of temperature. 2) Effect of solution annealing temperature on high-temperature tensile properties. 3) Stress to rupture strength at 350° and 400°C (660"to750°F). 4) Impact strength. 5) Electrical conductivity and resistivity as function of temperature. 6) Thermal expansion.

Jan 1, 1961

By R. H. Doremus, E. F. Koch

The first carbide phase that precipitates at 120°C from a iron containing about 0.02 wt pct, C was studied with the electron microscope. In both strained and unstrained material the carbide particles appeared to form on the dislocations in the iron, in agreement with the results of the kinetic study in part II. The structure of the carbide was tentatively identified as an expanded a-iron lattice (body-centered tetragonal) with about 0.7 wt pct C. This phase appeared to be metastable and apparently transformed into cementite or epsilon carbide when the iron was over-aged. WhEN a iron containing less than about 0.025 wt pct C is quenched from 700°C to room temperature the carbon is retained in solid solution and precipitates out slowly with time. The morphology and structure of the precipitating phase are still in doubt, two different carbide phases, epsilon carbide and cementite, have been identified, but there is considerable disagreement about the time and temperature at which they appear.1-4 Epsilon carbide seems to form at lower temperatures than cementite, although one group of investigators4 found only the latter phase over a wide range of aging temperatures. Usually these two phases have been identified after aging times much longer than needed to drain the carbon from supersaturated solution, at least for aging temperatures below 200oC. The precipitated carbides have been observed with the electron microscope,'-5 but again most results have come from samples aged much longer than necessary to reduce the carbon concentration in solution to a low value. In this study the carbide phases were observed in earlier stages of precipitation with the electron microscope, in order to learn more about the shape, size, and distribution of the carbide particles. Samples strained small amounts before aging, as well as unstrained samples, were studied, and the structure of the carbide phase was tentatively identified. EXPERIMENTAL "Ferrovac E" vacuum-melted iron, from which the wires for kinetic studies were also made (Refs. 6 and 7 and the following paper) was used for this work. An analysis of this material is given in Table I; it agrees well with the manufacturer's values. The number of inclusions in the iron was very small, as can be seen in the optical micrograph in the following paper. Pieces of iron about 1 mm thick and 5 to 10 mm in diam were used for all the studies except for those in which the sample was strained before aging; then the specimen was a rod 3 to 6 mm in diam and 20 cm long. The samples were held at about 700°C in wet hydrogen for at least an hour to remove residual carbon and nitrogen, after which they were heated to 950" (in the y region) and cooled to room temperature in the furnace. This treatment gave an average grain diam of more than 1 mm, so that the effect of grain boundaries on the precipitation process was negligible. The samples were carburized at 710°C for about 2 hr in hydrogen that had passed over toluene held at -30°C; then they were rapidly quenched into water. From chemical analysis this treatment gave a carbon concentration of from 0.012 to 0.016 wt pct, which is less than the solubility of carbon at this temperature. After quenching, the samples were aged at 120 "C in an oil bath for vari-

Jan 1, 1961

By H. S. Caldwell

Molten zinc, condensed from zinc vapor, was used by the Federal Bureau of Mines to leach aluminum from an aluminum-silicon alloy made by carbothermic reduction of silicious aluminum ores. Zinc requirements were minimized by re-fluxing condensed zinc in a low-pressure, Soxhlet-type distillation unit. The minimum ratio of zinc used to aluminum in the crude alloy was approximately 2:1. When the system pressure was reduced from atmospheric pressure to 100 microns or less, the rate of aluminum extraction increased by a factor of 20. Leaching rates were much higher when the zinc vapor was condensed directly on the crude alloy than when molten zinc was passed over the alloy in the absence of appreciable zinc vapors. Observations indicated higher extraction efficiencies from crude alloys containing greater amounts of iron. Complete extraction was obtained with negligible loss of zinc. Assuming complete removal of zinc, the aluminum products will contain 1 to 6 percent silicon and about 0.5 percent iron plus titanium. The leached crude-alloy residue is a highly friable spongelike material containing about 80 percent silicon, several percent iron and titanium, with the remainder aluminum. This extraction method has been patented (Patent 2,810,637) and assigned to the Government. Research and development investigations are continuing at the College Park Metallurgy Research Center.

Jan 1, 1961

By Frank Parrish

THIS REPORT by the Federal Bureau of Mines presents data on water-supply wells used by waterflood operators in North Texas and shows the distribution of permeable source sediments. Averages of well characteristics, including static fluid levels, working fluid levels, net thicknesses, producing rates, and depths, are presented and discussed. Essentially all water used in waterflooding is mineralized water from consolidated sediments. This study is concerned with the geology and distribution of these mineralized source sediments, whereas previous work in this area was predominantly a study of shallow sources of potable water. Tables, isopachous maps, and electric-log cross sections are included to describe the several source aquifers. In general, water-producing capacity increases with depth of the sediments. Wells completed in Cretaceous sediments 82 to 600 feet deep yield 50 to 600 barrels of water daily, whereas those completed in Pennsylvanian sediments 360 to 4,110 feet deep yield 100 to 7,000 barrels daily. Although deeper formations are used where oil and water are produced conjunctively and where large withdrawal rates are required, insufficient well data prevented mapping of deeper formations.

Jan 1, 1961

By H. Kenworthy

The purpose of the study described in this publication is to develop methods for recovering simple master alloys or single metal components from discarded and scrapped S-816 alloy, The Bureau of Mines started this investigation late in 1955 after the need became apparent for a method of reclaiming high-temperature alloys from an ever-increasing accumulation of rejected and wornout jet engine turbine buckets. Laboratory studies showed the following: (1) Pyrometallurgical separations are not selective enough, (2) several methods can be used for effective chemical dissolution of the major constituents of the alloy, (3) a master alloy or complex salts of cobalt and nickel can be separated, (4) chromium, contaminated by several other metals, may be segregated, and (5) more time and effort need to be expended in separating the minor constituents and improving the purity of the major metals removed. Difficult and incomplete chemical separations were attributed to the complexity of alloy composition, as were the long tedious chemical analyses o' products. For determination of several of the metallic components, standard methods of separation and routine analytical procedures had to be considerably modified to achieve satisfactory results. The overall technical problems involved in separating S-816 components do not appear to be insurmountable; however, refinement of several of the methods used in this investigation is desirable.

Jan 1, 1961

By J. E. Elliott, K. O. Miller

Solubility studies were carried out to establish the phase distributions for various Fe-Ni-Pb-C alloys at temperatures where the metallic components exist as liquid solutions. Temperature us composition diagrams for the Ni-Pb, Fe-Pb, Fe-Ni-Pb, and Ni-Pb-C systems are derived by employing various approximations in conjunction with the data. Results are summarized for 1550°C in a quaternary phase diagram of the Fe-Ni-Pb-C system. BECAUSE surprisingly little information has been published on the phase diagrams of the Ni-Pb, Fe-Pb, Fe-Pb-Ni, and Fe-Ni-Pb-C systems, a study of these systems was undertaken to ascertain the important phase relationships in the temperature range of 1300" to 1550°C. Measurements were also made on the carbon-saturated systems in the hope that they would assist in the interpretation of the systems without carbon. This paper reports the results obtained from the simple equilibration of the various liquid and solid phases. EXPERIMENTAL PROCEDURE The experimental technique involved holding appropriati quantities of the metals in an alumina crucible, or in a graphite crucible when saturation of the melt with carbon was desired, for sufficient time at the desired temperature to ensure equilibrium. Then a sample of each liquid phase presen was drawn into a small-bore silica tube. This sample was withdrawn quickly from the furnace, cooled, and sent to the chemical laboratory for analysis. The cell assembly used is shown in Fig. 1. Durin the work on the Fe-Pb-Ni system, it was placed in a furnace wound with 20 pct Rh-80 pct Pt wire. This furnace eventually failed and subsequent studies were carried out between 1350" and 1475°C in a tube furnace heated by silicon-carbide resistance elements. A protective atmosphere of argon with approximately 10 pct hydrogen was supplied to the cell assembly at a gage pressure of 1 in. of water. Hydrogen was passed over palladized alumina and then anhydrous calcium chloride for purification. Argon was purified of oxygen and water vapor by passing it over copper gauze at 550°C and then through a calcium chloride drying column. The gases were mixed and redried before they entered the equilibration cell. Temperature was measured by calibrated Pt/Pt-10 pct Rh thermocouples and a Rubicon Type B potentiometer. The thermocouples were standardized against the melting points of pure nickel

Jan 1, 1961

By Thomas C. Atchison

The experimental work described in this report is part of a continuing study by the Federal Bureau of Mines of the fundamental physical processes involved in breaking rock with explosives. Six explosives were tested for their strain-producing abilities in a dolomitic marble. The explosives selected for testing had a tenfold variation in detonation pressure and a fivefold variation in characteristic impedance (product of loading density and rate of detonation). Strain pulses produced by the detonation of small charges of the explosives were recorded at distances of 5 to 130 feet. Peak strain, ?, was found to decrease with distance, R, in accordance with an exponential propagation law previously determined for other rock types, namely ? = (K/R)e ?aR The absorption constant, a, did not vary significantly with the explosive and was of the same order of magnitude as that for other rock types. The different explosives produced a fivefold variation in the value of the intercept constant, K.

Jan 1, 1961

By Maurice J. Peterson

The applications of optical spectrochemical methods of analysis for determining trace impurities in metals are described, and the need for developing analytical procedures capable of accurately determining fractional parts per million of impurity elements in metals is stressed. Factors which determine sensitivity of detection and means to extend sensitivity levels in spectrochemical methods are discussed. Examples from the current literature illustrate the diversity of spectrochemical techniques that have been applied to the analyses of varied sample types, Many of the methods use preconcentration procedures to increase sensitivity limits. A bibliography containing abstracts of recent methods in included. Optical spectrochemical analysis is based upon the measurement of radiant energy emitted by atoms of the elements to be determined when a sample is subjected to a suitable source of excitation. The behavior of the valence electrons during excitation, usually by an arc, spark, or flame, produces radiant energy of specific wavelengths. This is recorded as spectral line images on a photographic film or plate by the spectrograph; for direct-reading instruments, the spectral lines are detected with photomultiplier tubes. The spectral lines result from the excitation of atoms in the sample. Each variety of atom produces its own characteristic set of lines, thus serving to identify the elements in the sample. Increased concentrations of elements in the excited sample results in increased blackening of the spectral line images.

Jan 1, 1961

By M. I. Copeland

The investigation of the zirconium-gadolinium equilibrium diagram was part of a program to investigate rare:earth alloys for use as nuclear reactor control materials. Investigation of the zirconium-gadolinium equilibrium diagram revealed a eutectic system with limited terminal solubilities and one peritectoid reaction. The eutectic composition occurs at about 82 percent gadolinium, and the eutectic isotherm, which occurs at 1,220 ±5° C., extends from about 12 to 99+ percent gadolinium. A peritectoid isotherm occurs at 890 ±5° C. and extends from about 2 to 99+ percent gadolinium. The solubility of gadolinium in beta zirconium decreases from about 12 percent at 1,220 ±5° C. to about 2 percent at 890 ±5° C. The solubility of gadolinium in alpha zirconium decreases from approximately 5 percent at 890 ±5° C. to between 2 and 3 percent at 600° C. Vary little solubility of zirconium in gadolinium was indicated. An allotropic transformation of gadolinium was observed at 1,260 ±5° C. A change of the gadolinium transformation temperature on alloying with zirconium was not observed.

Jan 1, 1961

By Oscar H. Lentz

During 1960, the controversy over percentage depletion reached the level of debate between presidential candidates. Nixon took the position that he would not tamper with the status quo in this matter. Kennedy took the position that he was willing to take a fresh look at the issues involved. Kennedy's position appears to have been based upon two premises: (1) new sources of federal revenue may be needed; and (2) current depletion rates, even if sound in principle, may be too high and, therefore, inequitable. The latter premise constitutes the basis for the claims that depletion allowances are simply "loopholes" of tax avoidance. Very probably the controversy over percentage depletion will remain in the political limelight during most of the coming decade. It is quite possible that the current depletion rates, at least those for oil and gas, will be reduced during this period. The aim of this paper is to isolate the complex causes of this mounting opposition to percentage depletion.

Jan 1, 1961

By David M. Gullikson

As part of its program of petroleum production research the Federal Bureau of Mines has long been engaged in the study and development of systems of analysis of oilfield waters (8, 12, 20, 21, 22, 27, 30).21 However, many of the early chemical procedures developed by the Bureau and widely adopted by the petroleum industry are time consuming, and some are unreliable for determining certain constituents found in California oilfield waters. Because of the need for more rapid and more accurate methods having greater sensitivity with low concentrations of some constituents, a study has been made by the Bureau's Petroleum Research Laboratory at San Francisco, in developing new techniques and modifying previously published techniques for analyzing oilfield waters by flame spectrophotometric, potentiometric, and colorimetric methods. Test solutions were synthesized for testing the suitability and accuracy of the procedures, and the effect of interfering ions. These solutions contained known quantities of characteristic constituents of oilfield waters including sodium, magnesium, potassium, calcium, lithium, strontium, barium, sulfate, chloride, bromide, iodide, carbonate, bicarbonate and borates in a wide range of concentrations. The compositions of these synthetic brines are listed in table 22. Many California oilfield waters contain salts of petroleum-derived organic acids and several synthetic oilfield waters also were prepared to which large quantities of naphthenates or salts of petroleum acids were added.

Jan 1, 1961