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MOUND LABORATORY PROGRESS REPORT FOR JANUARY 1961

Description: Work was begun to determine the physical properties of mica-filled diallyl phthalate. Both the impact and tensile strength values compared favorably wlth asbestos-filled DAP formulatlons. The tensile values compared with the upper limit tensile strength values for asbestos-filled formulations. Adiprene-ferric acetyl acetonate-polyol systems were developed as adhesives and their properties studied. Sources of kilogram quantities of Th/sup 2//sup 3//sup 0/ were investigated. The samples were analyzed by a direct CeF/sub 3/ precipitation procedurc or by a tributyl phosphate-cerium procedure. The half- life of Ra/sup 2//sup 2//sup 3/ was found to be 11.3700 plus or minus 0.0065 days. Differential thermal analyses were made of lanthanum and praseodymium metals. Three preilminary determinations of the density of molten cerium were made by the vacuum pycnometer method. An average value of 6.58 was obtained. Leaching tests in water and in 0.1N HCl were continued on fibers of an experimental glass containing 10 wt.%n plutonium oxide. (M.C.G.)
Date: January 31, 1961
Creator: Eichelberger, J.F.
Partner: UNT Libraries Government Documents Department

Mound Laboratory Monthly Progress Report for February 1961

Description: A survey and re-evaluation of previous work on polyurethane and polyurethane--epoxy copolymer systems was initiated to determine which phases are more productive than others. The effects of varying excess polyol content were studied. Work was carried out to define the amounts of butamediol that the system Adiprene L-213-ferric acetyl acetonate can tolerate and still be thoroughly cured. An experimental diallyl phthalate formulation was made and tested. A survey is being made of potential sources of kilogram quantities of Th/ sup 2//sup 3//sup 0/ in the United States. Analyses of various samples indicated concentrations almost three times as great as previously reported. The half-life of Rain was recalculated to include new data, and the results are reported as a function of the resolution time of the gas flow proportional counter. A method is being developed for determining the coincidence correction in porportional alpha counters by following the decay of a short-lived isotope. Additional determinations were made on the density of liquid cerium by the vacuum pycnometer method using tantalum pycnometers of about 0.5 cm/sup 3/ capacity. The viscosity of molten plutonium metal was investigated from 648 to 950 deg C with a cup viscometer. The construction of the hightemperature colorimeter was continued. Work was continued on the fabrication of plutonium-bearing glass fibers. (M.C.G.)
Date: February 28, 1961
Creator: Eichelberger, J. F.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY MONTHLY PROGRESS REPORT FOR MARCH 1962

Description: In research on plastics, flow curve data were obtained on asbestos- filled diallyl phthalate formulations. The tensile properties of adhesive formulations after 26 weeks cure time are being tested. In development of radioelements, progress is reported in investigations of kinetics invoived in Po(IV) reduction by ferrous iron and selective adsorption of trace elements. Development of separating and purifying processes is reported for Xe, H/sub 2/, and C. Work on the Ranger x-ray sensor was devoted to fiim casting techniques and Be metallography and deposition. Developmental work in Pu-bearing fuels is reported on techniques for differential thermai analysis, interfacial tension studies on liquids, cerium viscosity, Pu phase studies, and Pu-bearing glass. Developmental work in support of SNAP was devoted to welding, capsule design, source metallography, and recovery of U . Calorimetric measurements related to Ra/sup 223/ half life are reported. Development of a program for reduction of spectrometric data is also reported. (J.R.D.)
Date: March 30, 1962
Creator: Eichelberger, J.F.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY MONTHLY PROGRESS REPORT FOR MARCH 1961

Description: Adhesives. The effects obtained when diols and triols are used to cure Adiprene L-213 are discussed. Most of the formulations are very viscous and present difficulties in degassing operations. Ionium Project. Four plant samples having 1 ppm or more of Th/sup 2//sup 3//sup 0/ were analyzed for Th/sup 2//sup 3//sup 0/ in two different ways, one using HNO/sub 3/ digestion and the other using HClO/sub 4/ digestion. The difference between these two methods found for one sample is attributed to insolubility induced by calcining. Half Life of Radium-223. The decay of a purified Ra/sup 2//sup 2//sup 3/ sample was followed by alpha counting for 109 days; the results indicate that a long-lived impurity may be the cause of the nonconvergence of the probable error in the resolution time range. Purification of a composite sample containing Ac/sup 2// sup 2//sup 7/ to give a source of Ra/sup 2//sup 2//sup 3/ is described. Determination of Coincidence Correction. The coincidence correction was determined for a proportional alpha counter with Pb/sup 2//sup 1//sup 1/, and the best resolution times and half lives are given. Plutonium Alloy Research. The density of liquid Ce was measured from 825 to 1000 deg C with the vacuum pycnometer method; the thermal coefficient of cubical expansion is found to be very small, 33 x 10/sup -//sup 6/ cm/sup 3// cm/sup 3// deg C, and the volume change of fusion is also estimated to be small, less than 0.5%. The viscosities of molten La and Pr were determined from their melting points up to 996 deg C. Qualitative tests were made to study the wetting properties of Pu alloys on Ta. Pure liquid Pu did not wet Ta surfaces, but a Fu--43 at.% Co alloy had improved wetting properties. Plutonium-bearing Glass Fibers. Leaching tests were made at room temperature on ...
Date: March 30, 1961
Creator: Eichelberger, J.F.
Partner: UNT Libraries Government Documents Department

Calorimetry research progress report, March 1--31,, 1948

Description: Sixty-eight samples were assayed. The 5 calorimeters of type 30 were finished. Calorimeter 36, whose construction has been started, is an improved version of 30. A system of switches has been devised. A simple, fast, insensitive calorimeter for measuring high activity samples is being tested. The calculations on the half-life of postum were checked.
Date: December 31, 1948
Creator: Eichelberger, J.F.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY MONTHLY PROGRESS REPORT FOR JUNE 1961 ON CHEMISTRY

Description: Plastic Research. The tensile strength of Dacron-filled diallyl phthalate was determined to average 4377 psi. Composition and stress-strain data are tabulated for ten adhesive films. Analytical studies of an adhesive exudate are reported. Radioelements. Results of analysis of ioniumbearing raffinates and residues for Th/sup 232/ and of aged>s Ra/sup 223/ for Ac/sup 2/2/sup >/s7>s are given. Progress on Pa recovery from raffinates and residues and separation from Nb is reported. Isotope Separation and Purification. Proposed work on gas centrifugal and photochemical separation of uranium isotopes is discussed. Progress on xenon and helium isotopes separation and purification is outlined. Reactor Fuels and Materials Development. The density of liquid La at 945 to 1000 deg C was determined. The performances of an oscillating Cup viscometer with La and Bi and of a high-temperature calorimeter with Po/sup 210/ are described. A study of the compatibility of Haynes 25 alloy with Pu at 9O0 deg C indicated that very little penetration took place after the first hour at 900 deg C. The efficiency of escape of alpha particles from a glass fiber containing 10 wt% pu oxide was determined to be approximately 72%. Eight glass compositions were evaluated for their ability to dissolve 15 wt% Pu oxide at 1650 deg C. A glass neutron standard containing Pu and Be oxides was prepared. (D.L.C.)
Date: June 30, 1961
Creator: Eichelberger, J.F.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY MONTHLY PROGRESS REPORT FOR MAY 1961 ON PLASTICS, RADIOELEMENTS, ISOTOPE SEPARATION, AND REACTOR FUELS

Description: tems were cast and cured. Results of chemical tests on aa epoxy curlang exudate are included. Comparison of solvent effects on retention of radioelements by stainless steel was started and data are tabulated for Ac/sup 227/, Th/sup 227/, a nd Ra/sup 22//sub 3/. Work on protactinium was resumed after suspension of this project in 1960. Methods for preparation of small quantities of highly enriched U isotopes are being examined. Included in the survey are chemical exchange, electromagnetic separation, gaseous and liquid thermal diffusion, gas centrifugation, and photochemical techniques. Continued investigation of viscosities of La and Pr for use in Pu alcontinued along with studies of Pu bearing glass fibers. (J.R.D.)
Date: May 30, 1961
Creator: Eichelberger, J.F.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY PROGRESS REPORT FOR JULY 1963

Description: 8 7 6 2 ; 7 4 7 6 : 7 8 : : ; half life of 3.781 plus or minus 0.010 years based on calorimetric measuiements. The calorimetric assay of the sample will be continued ior several years to decrease the probable error. The decay scheme for /sup 209/Po--/sup 209/Po/ isitopic mixtures is being determined. The gamma spectrum is being studied using two sources of different isotopic composition. Definite peaks were established at 76, 260, 300, 575, and 9l0 kev. Various multiple coincidence experiments indicated that the 300- and 575-kev photons and the 76-kev x-ray are in triple coincidence. Relative intensities of the various gamma rays from the two different sources indicated that the 575-kev photon is associated with /sup 208/ Po decay, while the 260- and 910-kev states are attributed to /sup 209/Po. A theoretical estimate of the partial alpha half life for /sup 208/Po decay to the 2+ level in /sup 204/Pb (at 0.899 Mev) was made. This value (2.5 x 10/sup 6/ years) was determined graphically by extrapolation to an alpha particle energy of 4.2l1 Mev. /sup 209/Po--/sup 2o9/Po sources are being prepared for the investigation of the internal conversion electron spectra of these isotopes. Ion exchange techniques are being studied for the separation of /sup 227/Ac from / sup 227/Th, /sup 223/R a, and /sup 226/Ra. Naturally occurring lanthanum, thorium, and barium are being used as experimental substitutes. Composite elution curves indicated that lanthanum and /sup 232/Th can be successfully isolated with 2 M HCl, 3 M HNO/sub 3/, and ammonium acetate as elutrients. A purified form of the original Dowex 50W-X8 column packing matenial was used; the new material (AG-50W-X8) reduced tailing on the elution curves. /sup 228/Th was tentatively assigned a half life of 1.9132 years with an internal probable error of ...
Date: July 30, 1963
Creator: Eichelberger, J.F.; Grove, G.R. & Jones, L.V.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY PROGRESS REPORT FOR JUNE 1963

Description: 3 8 ; 9 4 5 7 5 C 9 E ; < : 7over a 1456-day period. The half life was calculated to be 12.355 plus or minus 0.0l0 years, based on measurements in three calorimeters. The yields of /sup 208/Po and /sup 209/Po from the irradiation of multicurie quantities of /sup 210/Po were calculated. Production of small quantities of /sup 208/Po and /sup 209/Po is possible by the (n,xn) reaction; however, large quantities of /sup 210/Po would be present in the /sup 208/Po--/sup 209/Po sample. On the basis of these calculations the maximum /sup 208/Po content would occur after 466 days' irradiation in the materials testing reactor. An experimental decay scheme was drawn for /sup 208/Po on the basis of experimental data. Experiments are in progress to determine whether levels at about 1.4 Mev in /sup 208/Bi are populated in the electron capture decay of /sup 208/Po The known half-life method for determining the resolution time of a counting instrument was found to yield only an average value for the counting range in the computation. To correct the counting error a series of computations should be made with data covering only a short segment of the decay curve rather than a single computation covering the entire range. Alternatively, the decayingpair method of half life determination can be used, eliminating the need for an accurate knowledge of the resolution time. A process for the separation of /sup 234/U from /sup 238/Pu was developed. One batch of feed solution was processed by the method, and 14 mg of / sup 234/U were recovered. A second continuous solvent extraction process is being investigated. Thermogravimetric studies and the differential thermal analysis of potassium plutonium suifate dihydrate were completed. The previously reported DTA thermogram for salt was confirmed. The existence of the complex ...
Date: June 28, 1963
Creator: Eichelberger, J.F.; Grove, G.R. & Jones, L.V.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY PROGRESS REPORT FOR MARCH 1963

Description: Using six hot-wire columns and three concentric tube thermal diffusion columns a cascade system was arranged to produce 0.04 g of 90% C/sup 13/ per day using methane as the feed gas-. The ten liter shipment of purchased methane enriched to 60% C/sup 13/ was received. This gas will be enriched to 90% C/slup 13/. Before removing the equilibrated gas from the concentric tube columns in preparation for using methane enriched in C/sup 13/ as feed material, a sample of methane taken from the bottom of the last column contained greater than 65% C/sup 13/. The hydrolysis of protactinium was found to be completely controllable and reversible and can serve as the basis for its separation from other elements, particularly its decay products. The tendency to hydrolyze is not a unlque characteristic of protactinium, but is exhibited, under appropriate conditions, by Th/sup 227/ and Ra/sup 223/ at trace levels. Traces of protactinium in 1N H/ sub 2/SO/sub 4/ can be removed from solution by a coarse glass wool filter through which the decay products pass readily. The reverse is true if the H/sub 2/SO/sub 4/ concentration is increased to 6N. The desorption of protactinium from platinum was a function of the reagent, the reagent concentration, and the amount of protactinium adsorbed. The relative solubility of protactinium in various reagents increased in the order: HNO/sub 3/ < HCl < H/sub 2/SO/sub 4/ < H/ sub 2/C/sub 2/O/sub 4/ < HF. Equations for computing the growth of the principal alpha-emitters in the Ac/sup 227/ decay chain were recalculated based on the recently redetermined half lives of Ac/sup 227/, Th/sup 227/, and Ra/sup 223/. Several laboratory experiments on waste disposal problems indicated that radioactivity levels in influent water can be significantly reduced by precipitating aluminum hydroxide as well as bismuth hydroxide in the ...
Date: March 30, 1963
Creator: Eichelberger, J.F.; Grove, G.R.; Jones, L.V. & Rembold, E.A.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY PROGRESS REPORT FOR NOVEMBER, 1963

Description: As a part of the effort to establish the vapor pressure of /sup 3/He as the international temperature scale between 0.3 and 3.2 deg K, the manometric contections from /sup 4/He to /sup 3/He are being determined. The results of a single run did not agree with the predicted values. Calculations indicated that a two to one thermal diffusion column cascade is more efficient than a three to one cascade for separation of neon isotopes. Gaseous impurities in neon were reduced from 3.40 to 0.26% by passing the impure gas through a charcoal trap at liquid nitrogen temperature. About 15 liters of gas containing 9% /sup 78/Kr and /sup 80/Kr were accumulated. Calculations to determine the shape factors for the thermal diffusion system were completed. A six-stage cascade system was converted to an eight-stage cascade system of ten hot-wire and concentric-tube columns. Prior to the conversion the sixstage system enriched natural methane to 74%. Additionally, 74% of that enriched methane product was mass 17. The concentric-tube columns completed the purification of a commercially enriched methane from 60% to over 90% /sup 13/C in the total carbon, About eight grams of the methane product were accumulated. A method was developed for fabricating threshold detectors by sealing them in copper cans. Twenty-two plutonium threshold detectors, returned because of high wipe counts, were removed from the aluminum cans; then the detectors were sealed inside copper cans by tungsten inert gas welding. The recanned threshold detectors had zero wipe counts. The erratic behavior of /sup 140/Ba- /sup 140/La was traced to a macroscopic impurity in the stock solution. A separation of this impurity by cation exchange indicated tentatively that it is stable strontium. The multiple source method for determining coincidence correction was compared with the double source method. The multiple source method offered no ...
Date: November 30, 1963
Creator: Eichelberger, J.F.; Grove, G.R. & Jones, L.V.
Partner: UNT Libraries Government Documents Department

A Calorimetric Determination of the Half Life of Polonium-210 (Final Report)

Description: Six determinations have been made of the half life of polonium with four different steady-state, resistance-bridge calorimeters and five different samples of polonium. These six values of the half life have been weighted and combined to give a grand-mean value of the half life of 138.4005 + - 0.0051 days.
Date: February 10, 1953
Creator: Eichelberger, J. F.; Jordan, K. C.; Orr, S. R. & Parks, J. R.
Partner: UNT Libraries Government Documents Department

Mound Laboratory Progress Report for December, 1964

Description: This monthly report has the following sections: (1) Radioelements - Uranium-234, Hydrolytic Separations of Protactinium, Polonium-208 and Polonium-209; (2) Isotope Separation and Purification - Carbon-13, Helium, Neon, Argon, Krypton, Xenon, Thermal Diffusion Research, and Helium Research; (3) Analytical and Instrumentation - Neptunium Analysis, Cobalt Analysis, Analysis of Enriched Uranium-234 for Comparison Purposes, Analysis of Stearic Acid in Silver Powder, Nuclear Magnetic Resonance Studies, Semiconductor Radiation Detectors, and Calorimetry.
Date: December 21, 1964
Creator: EIchelberger, J.F.; Grove, G.R. & Jones, L.V.
Partner: UNT Libraries Government Documents Department

Mound Laboratory Progress Report for September 1963

Description: Three silicone-based conductive adhesives were formulated and evaluated. One of the formulations had a resistivity of 0.089 ohm-centimeter after aging one week. After the same period the other two formulations had resistivities of 0.871 and 38.0 ohm-centimeters, Erratic adsorptive behavior of / sup 140/Ba was traced to in impurity in the Ba--/sup 140/La stock solution. Repurification by cation exchange did not improve the reproducibility of the separations, possibly because impurities are reintroduced by the distilled water. Definite improvement was noted when the /sup 140/Ba was separated from /sup 140/ La and other hydrolyzable materials by residue adsorption methods. A calorimetric measurement of a salt sample over a period of 148 days gave a tritium half life of 12.361 plus or minus 0.028 years. This value confirmed the earlier value of l2.355 plus or minus 0.028 years. The /sup 208/Po--/sup 209/Po mixture returned from Argonne National Laboratory is being processed further. Two batches of polonium-contaminated organic material were wet-ashed in nitric and perchloric acids. Further purification will be by techniques similar to those presently used for separating /sup 210/Po from bismuth. An unidentified gamma activity was found in the polonium that was recovered from pieces of Monel fluorination apparatus. The optimum conditions for decontamination of polonium process waste are being determined. Ferric sulfate was dissolved in the solution, and the pH was adjusted to a value between 7.0 and 12.0 to precipitate ferric hydroxide. However, the alpha and beta activity was not decreased sufficiertly to allow dumping of the wastes without further processing. A method of separating /sup 227/Ac from a mixture of its daughter products and /sup 226/Ra is being developed using ion exchange and solvent extraction techniques. Substituted elements are being used to evaluate the separation procedures prior to the separation of the radioactive isotopes. More than 99% of ...
Date: September 30, 1963
Creator: Eichelberger, J. F.; Grove, G. R. & Jones, L. V.
Partner: UNT Libraries Government Documents Department

Mound Laboratory Progress Report for May 1963

Description: Progress is reported on research directed toward. the development of adhesives, which are compatible with explosives; the measurement of nuclear properties of polonium isotopes; residue adsorption; separation and purification of isotopes; thermal diffusion theory analyses; emission strength analyses for neutron sources; and krypton-85 counting methods development. (B.O.G.)
Date: May 31, 1963
Creator: Eichelberger, J. F.; Grove, G. R.; Jones, L. V. & Rembold, E. A.
Partner: UNT Libraries Government Documents Department

MOUND LABORATORY PROGRESS REPORT FOR JUNE 1962

Description: Research and development progress is reported on plastics, analytical methods, radioelements, isotope separation and purification, reactor fuels and materials developmert, Ranger x-ray sensor program, and SNAP a. (M.C.G.)
Date: June 29, 1962
Creator: Grove, G.R.; Jones, L.V. & Eichelberger, J.F.
Partner: UNT Libraries Government Documents Department