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By A. H. C. A. Zimmerman

WE have just heard what must be regarded as a thoughtful, constructive and somewhat painful analysis of the financial function of our industry. While thinking about this, it is interesting to reflect on the conditions which have stunted the growth of the financial side of our affairs. Mining must be regarded as a wealthy business. •while immeasurable grub takes and development budgets have been lost, there can be little argument that a productive ore-body nearly always produces the type of wealth that breeds some extravagance. I recognize that this statement can be attacked from many sides, but an historical comparison with a commercial enterprise involving similar investment will demonstrate what I mean. However, these old times are be-ginning to disappear for a variety of reasons. High amongst these are: ( l) Increased costs of exploration. (2) Remoteness of many new finds. (3) Fixed or declining metal prices (particularly when expressed in constant dollars). ( 4) Constant demands for higher wages.

Jan 1, 1962

By P. H. Riordon

ONE OF the major sources of the world's supply of asbestos lies in a belt of ultrabasic rocks stretching through the Eastern Townships of Quebec where chrysotile asbestos has been mined continuously since 1878. The productive portion of the belt extends from the town of Asbestos in Shipton town-ship northeastward some 60 miles to the eastern edge of Broughton town-ship. (See map). Twelve mines, currently treating an aggregate of over 60,000 tons of rock daily, produce more than one million tons of asbestos :annually. An equal number of mines are now dormant, having for the most part exhausted their reserves. It is evident from the past and present activity, in this belt that it can look forward to at least half a century or more of large scale production. The host rock to the asbestos de-posits is essentially a peridotite which originally contained I 0 to 15 per •cent pyroxene. The peridotite, associated with dunite, pyroxenite

Jan 1, 1962

By J. B. Malcolm

The discovery of tungsten-bearing quartz outcroppings in Vance County, N. C., by the Hamme brothers in 1942, made international news in the mining industry and was, in fact, one of the major ore discoveries made in the U.S. during the last 25 years. Operations began at the Hamme mine in 1942, but after 16 years of successful operation, the mine was closed down in 1958 under adverse market conditions. By that time, it had produced nearly 20 million lbs of metallic tungsten. Because of the square-set timber mining method then in use, mine operating expenses were high, actually representing 78% of the total operating expenses at the property. In timber work alone, 160 men were employed. Approximately 500,000 bd ft of timber were placed monthly at a direct supply cost of $1.00 per ton of ore mined. Late in 1959, following a slightly improved position in the tungsten market, company management decided that, by changing the mining method, the operation could be economically feasible. The major premise in this decision was that a reduction of from 25 to 30% of the mining costs could be achieved by the conversion of the mining method from square-sets to horizontal cut and fill. Reopening of the mine began in February 1960, Full production has now been reached and overall mine productivity has been doubled.

Jan 1, 1962

By D. Mizer, J. B. Clark

In a recent investigation of the entire magnesium-yttrium phase diagram, Gibson and Carlsonl report the maximum solid solubility of yttrium in magnesium as 8.0 wt pct Y at 1050°F (565°C). However, independent studies of the precipitation in magnesium-yttrium alloys, 2 conducted prior to the publication of the above phase diagram, indicated a greater solid solubility of yttrium in magnesium. Accordingly, the magnesium-rich region of the diagram was re-investigated to determine more accurately the liqui-dus, solidus, and solvus of the magnesium solid solution in this system. Metallography and thermal analysis were chosen as the best corroboratory methods for accurately determining this region of the diagram. A magnesium-yttrium master alloy was prepared from yttrium of 99.9 pct purity and singly sublimed magnesium of 99.9 pct purity. Subsequently, the twelve magnesium-yttrium alloys shown in Fig. 1 were prepared using standard alloying procedures for magnesium. Metallographic samples of the alloys were heat treated under an SO, atmosphere in an electric furnace capable of control within ±3oF of the desired temperature. Alloy samples for the metallographic determination of the solvus, and for the precipitation studies were solution treated at 1000° F for 16 hr. Subsequent aging times for the solvus determination varied from a minimum of 6 hr for the higher temperatures up to 816 hr for lower temperatures. Periods of 30 min at temperature were used to generate liquation for the metallographic placement of the solidus and eutectic horizontal. The liquidus and the eutectic horizontal were determined by thermal analysis. Simple time-temper- ature heating and cooling curves were obtained from 10-g alloy samples heated and cooled in a well-insulated electric furnace. An Iron-Constantan thermocouple was placed in direct contact with the sample. The thermocouple did not contaminate the alloy sample since metallographic examination showed that the alloy melt did not wet or attack the thermocouple. The heating and cooling rates were approximately 5 to 8OF per min. The standard metallographic procedures for magnesium were used in polishing and etching the magnesium-yttrium alloys studied. Glycol etchant* was etchant was used to reveal precipitate in the solvus determination. The redetermined magnesium-rich region of the magnesium-yttrium diagram is shown in Fig. 1. The

Jan 1, 1962

By D. J. Bauer

A pure scandium solution was concentrated from 10-4 mole per liter to 0.5 mole per liter by continuous foam fractionation in a spaced, packed column. Recovery in the foam was 77 percent using a spaced, packed draining column with sodium n-methyl-n-"coconut oil acid" taurate as the surfactant. The technique was first studied batchwise in a small unpacked column to determine the more important variables. Optimum surfactant concentration was found to depend on scandium concentration. Extraction and, in general, enrichment ratios were highest in the 2.5 to 3.5 pH range at temperatures ranging from 50° to 70° C. An airflow rate of 136 ml./min. was satisfactory in the equipment used.

Jan 1, 1962

By John C. Machisak

The National Safety Competition is sponsored and conducted annually by the Bureau of Mines, U.S. Department of the Interior, to give greater impetus to the building of programs safeguarding the employees of the mineral industries from disabling work injuries. The results of the 1960 National Safety Competition are presented in this publication. Mines and quarries that were awarded the Sentinels of Safety trophy for the best safety record in their competitive group and those mineral operations that ranked second, third, fourth, and fifth in the competition are listed with a summary of their achievements in preventing disabling work injuries. In addition, this publication presents statistical data on disabling work-injury experience in all other mines and quarries participating in the annual competitions.

Jan 1, 1962

By Philip D. Anderson, Ralph Hultgren

Heat contents of extremely pure iron were measured over the range 300"to 1433"K, using a diphenyl ether calorimeter. Results from three samples containing widely differing impurities agreed with one another and with Previously reported results at higher temperatures (1184 ° to 1809°K) by Olette and Ferrier. From these data a table of heat contents of iron has been Prepared which is believed to be more accurate than those previously available. CP values have been derived which are consistent with these heat contents, with the best experimental Cp data, and with the thermodynamic conditions of equilibrium between bcc and fcc iron. The opinion is expressed that low-temperature extrapolations of presently known Cp values for y-Fe are not reliable. It would seem that the thermodynamic properties of iron, which is by far our most important metal, should have been well established long ago. This is not the case, however. As discussed by Olette and Ferrier,' there is objection to every earlier heat content measurement. While the best true Cp determinations agree well at temperatures below the Curie point, there is wide divergence at higher temperatures. Several investigators have examined available data and attempted to calculate thermodynamic functions for iron that are consistent with the two equilibrium temperatures of bcc and fcc iron. The two primary efforts were those of Austin' in 1930 and Darken and smith3 in 1948. The recommended values differ considerably; integration of Austin's Cp values leads to a heat content at 1100°K which is 300 cal per g-atom higher than the value recommended by Darken and Smith. The compilation of Fisher4 in 1949 was based on the selection of Austin. In 1956, Weiss and Tauer obtained yet another set of values by resolving Cp values into components due to dilation, lattice vibration, electronic excitation, and magnetism. The magnitude of contribution by each component and its dependence on temperature was estimated by semiempirical means. Their values are not self-consistent in that they do not form smooth curves when plotted vs temperature; moreover, their calculations cannot easily be repeated since they do not give the values of some of the parameters used. Clearly, experimental values for iron were in a most unsatisfactory state. The presently described measurements of the heat content of iron were therefore undertaken, covering temperatures as high as 1433°K. While the work was in progress, the high-temperature (1193" to 1789"K) heat content measurements of Olette and Ferrier' were published; in the region of temperature overlap the present results agree with Olette and Ferrier well within experimental accuracy. It is believed that the present results, combined with those of Olette and Ferrier, provide for the first time a reliable set of heat contents of iron from room temperature to the melting point. From these data, guided by available Cp measurements, it proved possible to derive Cp, entropy, and free energy function values for @-iron from room temperature to the melting point, and for y- iron in the temperature region of its stability. Exhaustive study led to the conclusion that extrapolations of y-iron functions to room temperature were not reliable enough to be useful; hence these have been omitted from the tables. EXPERIMENTAL Materials. Three samples of extremely high purity iron from different sources, containing widely different impurities, were measured. The first of these, designated "Chipman", was kindly supplied by Dr. K. K. Kelley of the U. S. Bureau of Mines from a lot which was made many years ago by Dr. John Chipman of the Massachusetts Institute of Technology. The second, designated6'Teddington", was supplied by the National Physical Laboratory, Teddington, England, from a lot zone-refined by them. The third sample, designated "Irsid", was supplied by the Institute de Recherches de la

Jan 1, 1962

By L. O. Bacon

This Bureau of Mines report summarizes the results of laboratory work in the design of instrumentation for obtaining the dynamic tensile strength of rock at minimum loading. Minimum loading is defined as the lowest tensile loading by pulse reflection to cause fracturing. The instrumentation for obtaining dynamic tensile strengths of rock cores evolved into the use of a compressed-air pellet gun to impact one end of a rock core, suspended by wires, at increasing increments of air pressure. Maximum strain was measured on most or all of the impacts, and the strain at fracture of the core was obtained by extrapolating the pellet velocity-strain curve to the pellet velocity at fracture. Stress at tensile fracture was obtained from the maximum s train, and the dynamic Young's modulus was calculated from the rod velocity by using simple rod theory.

Jan 1, 1962

By E. J. Ostrowski

The history of ironmaking dates back to 4000 BC when an open forge was used to produce a sponge iron from a heap of ore and charcoal. Even at this early date, man recognized the need for a fuel and a reducing agent. As time passed, man developed new methods of producing iron; however, these developments were centered on the mechanical aspects, and as a result, a furnace evolved which is now known as a blast furnace. During this period of evolution,' man struggled with the only fuel he knew - charcoal. Some 5600 years passed before any attempt was made to use coal as a fuel for the blast furnace. The use of coal had its beginning in 1619 when Dud Dudley of England first attempted its use in the blast furnace; as a-fuel and as a reducing agent. Coal charged to the top of the blast furnace was not satisfactory. The volatile matter of the coal choked the flues, and also the poor, strength qualities would not support the weight of the ore. Breaking up of the coal compacted the stock column to an impervious mass. One hundred and sixteen. years later in 1735, Abraham Darby of England introduced coke as the fuel and reducing agent in the blast furnace. The acceptance of coke as a fuel for the blast furnace was not spontaneous. As late as 1870, one-half of the pig iron product of the United States was made with anthracite coal, 30 per cent with raw bituminous coal and coke, and 20 per cent with charcoal. However, by 1910, 96.2 per cent of the blast furnace product was made with coke, 2.4 per cent with anthracite and coke admixture, and 1.4 per cent with charcoal. Coke became the standard fuel in the blast furnace. As the art of ironmaking progressed, more pig iron was produced and more coke was consumed. Coke oven capacity was progressively increased. In 1910, there existed approximately 4,000 coke ovens; in 1960 there was approximately 15,000 ovens. This increase in coke oven capacity was necessary to feed the mammoth appetite of modern blast furnaces.

Jan 1, 1962

By J. H. Waxweiler, L. C. Ikenberry, R. J. Bendure

Carbon which is present as insoluble carbides in austenitic stainless steels can be measured quantitatively by dissolving the steel in iodine-methanol and analyzing the residue for carbon. Severe sen-sitization was observed in Type 302 due to precipitation of only 0.003 pet carbon. Both cold work and the presence of delta ferrite caused a marked acceleration in rate of carbide precipitation. Carbide precipitation rates in 17-7 PH were stzulied for the austenite conditioning and also the aging heat treatment. CARBON and its compounds exercise a major influence on the properties of stainless steels and their response to thermal treatment. Sensitization in 18-8 type stainless steels has been the subject of numerous investigations throughout the years. Bain, Aborn, and utherford," and Binder, Brown, Frankss all studied the effects of heating austenitic stainless steels in the temperature range of 1000° to 1500°F. The primary purpose of most of these studies was the investigation of susceptibility to in-tergranular attack in acids due to these sensitizing heat treatments. Intergranular precipitation of carbides was always associated with intergranular attack but it was recognized2 that severe attack could occur with but minute quantities of precipitated carbide. Mahla and ielsen utilized the electron microscope to make a significant contribution in illustrating the appearance and method of growth of chromium carbides during sensitizing heat treatments. However, as they stated, their studies of residues could not be used to obtain a quantitative measurement of the amount of carbon which was actually precipitated. The aim of the present investigation was to devise a relatively fast, simple method for the quantitative measurement of carbides in stainless steel. EXPERIMENTAL WORK The initial investigations were made to determine the best means of separating carbides from the matrix. A number of dissolving media were tried using both chemical and electrolytic attack. Qualitative examination of the extracted residues by X-ray diffraction indicated that solution in iodine-methanol would furnish a good means of separation. Consequently, further work was pursued along this line. The method is quite simple. The sample in the form of millings or nibblings is dissolved in iodine-methanol solution at room temperature (6-g iodine, 25-ml methanol per g of sample). The insoluble residue containing the carbides is separated by suction filtration through an ultra-fine glass filter disc. This is a very fine filter medium that will retain particles as small as 0.1 to 0.2 p in diameter. After washing with methanol and drying, the filter disc and residue are placed in a conventional combustion carbon-tube furnace and the carbon determined gravimetrically. Using this technique it was found that reproducible insoluble carbon values were obtained. However, since such small amounts of insoluble carbon were obtained on Type 302 after sensitizatipn at 1250°F and 1500°F, the values were confirmed by a second method. In the second method the sample was dissolved with copper potassium chloride and filtered through a millipore paper. This treatment dissolves the matrix but leaves undissolved practically all of the carbon irrespective of how it is present in the steel. The amount of insoluble carbon present as chromium carbide is determined by calculation from the analysis of the residue for chromium and iron. The derivation of the formula used for this calculation is discussed later. The values obtained by the indirect copper-potassium-chloride method were in agreement with those obtained by the iodine-methano1 method. See Table I. It should be pointed out that the sensitivity of the direct combustion method is not too high when the amount of carbide present is small. This is due primarily to inherent blanks and to analytical errors such as weighing. For this reason it cannot be stated with any degree of certainty that there is a significant difference between values of 0.002 and 0.005 pct. Having confirmed that the iodine-methanol extraction gave a quantitative measurement of the precipitated carbides in Type 302, exploratory tests were conducted on Armco 17-7 PH stainless steel. Samples from commercial Heat 54807 were solution annealed at 2000°F, water quenched and heated at 1250" and 1500°F, and water quenched. The analysis of Heat 54808 is as follows:

Jan 1, 1962

By H. O. Seigel

Induced Polarization includes many types of dipolar charge distributions set up by the passage of current through consolidated or unconsolidated rocks. Among its causes are concentration polarization and electrokinetic effects in all rocks and the phenomenon of Overvoltage in rocks containing electronic conductors such as metallic sulphides and graphite. In normal rocks the polarization effects may be usually con-fined within relatively narrow limits and any large departures may be at-tributable to the presence of electronic conductors. In practice, Induced Polarization is measured in one of two ways. In the first a steady current of some seconds duration is passed and abruptly interrupted and the slowly decaying transient voltages existing in the ~round are measured after interruption. This is known as the "pulse", "transient", or Direct Cur-rent Induced Polarization (D.C.I.P.).The second method entails a comparison of apparent resistivities using sinusoidal alternating current of two or more frequencies, generally within the range of 1/10 to 10 c.p.s. Induced Polarization extends the

Jan 1, 1962

By E. W. Lucht

THE term "high pressure", as used in industry today, is applied rather loosely. Generally, it refers to pressures that are higher than those encountered in most industrial processes although no definite limits are normally stated. For the purpose of this talk I should like to set rather arbitrary limits to the term "high pressure", and in ab-solute figures this would be the range from 1000 psi to perhaps 40,000 or 50,000 p.s.i. The scope of high pressure technology is very broad, and it would take more time than we have avail-able here today to cover fully even one aspect of the field. Therefore, I should like to discuss just some of the techniques used and problems en-countered in high pressure operations. Research work into the high pressure region dates back about 150 years, but it was not until 1910 that the first commercial application of high pressure technology was made in the production of ammonia.

Jan 1, 1962

By A. G. Loomis

METHODS for measuring relative permeability as a valid function of saturation were compared by the. Bureau of Mines, using core samples from representative oil-productive California formations, from the Bartlesville sand in Oklahoma, and from synthetic samples. Measurements for gas-oil systems were made by steady-state dynamic, unsteady-state displacement and two stationary-phase methods. Measurements for water-oil systems were made by the unsteady-state displacement method. As the ratio rather than individual relative permeabilities is measured by the last method, three methods for calculating individual relative permeabilites from their measured ratio were compared for gas-oil systems and two methods for water-oil systems. Errors arising from capillary discontinuities, such as the end effect and stabilized-zone flow, are discussed and evaluated; possible errors rocs arising from turbulant flow are also examined. The inapplicability of non-steady-state methods for water-oil systems that are not definitely oil-wet is discussed in detail. Measurements of relative permeability to both gas and oil can be made quickly and accurately by the steady-state dynamic method when rates of flow of the two phases are sufficient to minimize the capillary discontinuity at the outflow end of the sample. At such rates relative permeability-saturation measurements are essentially independent of the rate of flow. The steady-state method wits modified by a dispersion section at the inflow end of the sample acid designated tie dispersed-feed method.

Jan 1, 1962

By M. J. Langley

Zinc ores were first discovered in Tennessee in 1856 at Jefferson City where a deposit of oxidized ore became known as the Mossy Creek Mine. From that time until 1913 small scale attempts at prospecting and mining were made in various parts of the district. The actual systematic development of the zinc deposits dates from 1913 when the American Zinc Company started operations at Mascot. Six mines are in operation by three companies and a seventh mine is being developed by a fourth company. The total daily production from the field is 11,000 tons of crude ore, which grades from 3 to 6 per cent zinc. Most of the ore bodies are large and ramiform, resembling asyrmetrical networks in which the ore shoots form channel like branches with areas of non-comercia1 rock, called blank islands. Most of the orebodies are adapted to large scale mechanization.

Jan 1, 1962

By B. S. Tani, R. V. Schablaske, M. G. Chasanov

In the Ti-Cd system two intermediate phases, TiCd and Ti Cd, have been found and characterized by X-ray diffraction powder techniques. An earlier reference' had reported the existence of the compound Tisd. No structural details, however, were given nor was there any indication of the possible existence of other binary compounds. Studies of the solubility of titanium in liquid cadmium2 led to the discovery of both TiCd and Tisd. The solid phase in equilibrium with saturated solutions of titanium in liquid cadmium at temperatures below 620°C is TiCd, whereas TizCd is the equilibrium solid phase above 620°C. Both thermal analysis and X-ray studies show that a peritectic reaction between the y phase (~isd) and cadmium to form the 6 phase (Ti Cd) occurs at 620°C. X-ray diffraction powder photographs of material isolated from the ingots used in the solubility measurements as well as material prepared by a direct heat of the appropriate stoichiometric amounts of titanium and cadmium can be indexed on the basis of a tetragonal unit cell with a = 2.904 ± 0.002A, co = 8.954 * 0.004A, c/a = 3.083. No variation of lattice parameters indicative of a range of composition is evident. With four atoms in the unit cell the calculated density of the intermetallic is 7.05 g per cm3; the observed value is 7.07 g per cm3. The TiCd lattice is primitive as indicated by the fact that there are no systematic absences among hkl reflections. The absence of all hko reflections for which h + k = 2n + 1 is also evident. This systematic absence indicates the following two space groups, C\h — P4/n and D&~4/nmm; both groups, however, have the same two- and four-fold positions. Stoichiometry, symmetry and space group indicate two likely structure types. They are the PbO-litharge3 (B10) type and the Ti CU (B11) type. Spatial considerations favor the B11 structure with atoms placed in the following positions: 2Ti (c) 0, 1/2, Z; l/2, 0, Z 2Cd(c) 0, 1/2, Z; 1/2, 0, Z The TiCd structure may be summarily described as a layered structure in which double cadmium layers alternate with double titanium layers along the c-axis. The best agreement between calculated and observed intensities is obtained for the values ZTi = 0.608 and ZCd = 0.130. Calculated and observed powder intensities as well as other pertinent powder data are recorded in Table I. Interatomic distances for the proposed structure are recorded in Table II and are to be compared with the distances of closest approach for titanium and cad-

Jan 1, 1962

By A. B. Whitehead

A spectrographic method for the determination of 18 impurities in cerium is presented. The carrier distillation technique is utilized to separate the spectra of impurities from the complex spectrum of cerium. Metal samples are ignited to the oxide, mixed with silver chloride carrier containing an internal standard, and excited with a 20-ampere direct-current arc. An additional exposure, made after carrier depletion, provides for the determination of refractory elements. Experiments to determine the best carrier, sample-carrier ratio, electrodes, arc current, exposure conditions, internal standards, and any matrix effect are described. The relative standard deviation of the method at the 20- and 200-part-per-million levels is about 25 and 15 percent, respectively. The average relative error is about 20 percent in the 10- to 1,000-part-per-million concentration range.

Jan 1, 1962

By Paul M. Clifford, David M. Baird

The Great Northern Peninsula of Newfoundland consists of a Precambrian core of gneisses and granitic rocks, cut by numerous diabase dykes. This complex is surrounded by an envelope of sedimentary rocks of Cambrian to Carboniferous age. Radiometric dates from two granite masses in the core give a mini-mum age of -945 m.y. (Grenville) for the last major tectonic activity. This Grenville deformation conferred upon the core substantially its present structure which has controlled later events to a marked degree. Block movements of the core, dominantly in a vertical sense, have ex-posed it to erosion at intervals. The nature and distribution of the flanking sedimentary rocks and the present relief of the peninsula suggest four such movements. THE Great Northern Peninsula extends some 150 miles north-northeast from the northwest corner of the main body of the island of Newfoundland. It separates the Gulf of St. Lawrence from the Atlantic Ocean, except for the 12 mile wide

Jan 1, 1962

By M. M. Fine

This report describes a Bureau of Mines technical feasibility study of simultaneous reduction and induration of pelletized iron ore to make a product with superior qualities as blast-furnace feed. Highly reduced, physically competent pellets can be made from magnetite and specularite concentrates that contain small additions of bentonite as binder. In batch tests, pellets were dried, surrounded with solid fuel in crucibles, and heated to the reducing temperature. Total iron content of the best products was higher than 80 percent and crushing strength of 1/2-inch metallized pellets ranged up to 600 pounds or more. Comparative tests of several commercial oxide pellets showed a wide range in crushing strengths, but most values were less than 350 pounds. Continuous tests in a rotary kiln resulted in the same degree of reduction, but the pellets had lower crushing strengths because of the limitations in the maximum operating temperature of the small kiln.

Jan 1, 1962

By J. A. Harrison

Most coal being used in the United States has been subjected to one or' more processes of coal preparation. The physical and chemical characteristics of a coal have a marked influence on the ultimate uses that coal may have. The selection of the proper preparation processes may similarly be important in producing the best practical coal product for any particular use. The physical composition and distribution of physical constituents in the coal will partially determine the efficiency of the preparation process chosen and conversely distribution and concentration of coal macerals will, to a degree, be controlled by the preparation process. A number of preparation processes have been evaluated to determine this interrelation. If a coal having' certain specifications is desired, these evaluations trill assist in providing information needed for the production of this coal.

Jan 1, 1962

By A. A. Berk

The Bureau of Mines devised a test nipple for the field study of corrosion in the condensate-return lines of Federal heating plants. Corrosion surveys, made with this device, showed that the deterioration of the piping was caused principally by carbonic acid in the steam condensate. Corrosion problems were brought under control when the carbonic acid concentration in the condensate was decreased. In many instances, this was effected by decreasing the total carbon dioxide content of the feedwater; in others, the condensate acidity was neutralized with volatile, alkaline chemicals. Filming treatment with octadecylamine, reported successful in controlling return-line corrosion in industry, was much less effective in Federal area-heating plants. Laboratory study by the Bureau disclosed that octadecylamine is unstable in heating systems. Analytical methods were developed for this chemical and its degradation products in heating-plant condensate. Field surveys, in using these methods, confirmed the instability of the filming material. Laboratory tests showed that the degradation products are not useful film formers. Since filming treatment has little effect on condensate corrosivity, the piping was corroded where it was not coated by the treatment chemical.

Jan 1, 1962