ANALYTICAL CHEMISTRY DIVISION ANNUAL PROGRESS REPORT FOR PERIOD ENDING DECEMBER 31, 1960

Technical Report · Wed Feb 15 00:00:00 EST 1961

DOI:https://doi.org/10.2172/4093642· OSTI ID:4093642

Analytical Instrumentation (X-10). Work was continued on in-line instrumentation. Gamma-absorptiometric techniques for the continuous determination of heavy elements in flowing streams were studied. A plant type alpha -detecting instrument, designed to monitor for excessive product losses in chemical-processing waste streams was found to have sufficient sensitivity for the streams being considered at present. An absorption-cell attachment for a Welch Densichron reflection unit was designed and fabricated so that either reflectance or absorbance measurements can be made remotely. An automatic-fill circuit and a plunger-position . indicator were added to the control unit for the remotely servo-controlled pipetter. Development has continued of a high- resolution high-sensitivity, scanning, recording flame spectrophotometer. A corrosion-resistant pipet was designed and tested, and one was installed in a remotely servo-operated pipetter in the High-radiation-level Analytical Facility. The performance of the ORNL controlledpotential a-c polarograph was studied. Circuitry for counting drops from and measuring the rate of flow of mercury through a D.M.E. was designed and built. Derivative polarography provides a rapid, easy, and accurate means of determining n values. A standard addition method for the mathematical analysis of interfering derivative waves was developed; the method makes possible the correct measurement from interfering derivative waves of concentrations of the reducible species. Ionic Analyses (X- 10). Continued work in electrochemistry, titrimetry, spectrophotometry, and gas chromatography is reported. The technique of generation and back-titration of intermediate reagents by means of controlled-potential coulometry was studied. A method for the coulometric titration of uranium(lV) was investigated. A study was made of the chemical reaction between Purex waste solutions and sodium chloride. A method was developed for the titrimetric analysis of mixtures of monobutyl-, dibutyl-, and orthophosphoric acids. Spectrophotometric techniques are being developed for the fundumental study, at high temperatures and pressures, of aqueous solutions of interest in high-temperature chemistry and in reactor technology. An ultraviolet --visible --near-infrared spectrophotometer, designed to be operated at temperatures as high as 330 deg C and pressures of at least 3000 psi in the presence of high levels of alpha radiation, is being designed. A mathematical technique that uses high-speed digital computation was developed to resolve seriously overlapping spectral bands and fine structure. The gas chromatographic work was concerned with the analysis of gases from offgases of dissolvers and of HRT shield gas, with studies of the recombination of deuterium and oxygen in thoria slurries and with studies of radiolytic decomposition of water. Nuclear Analyses (X-10). Trace and macro quantities of many elements were determined in many types of materials by neutron-activation analysis; a summary of these applications is presented. In addition, other nuclear techniques, for example, neutron absorption, neutron transmission, and delayed-neutron counting, have been used to determine concentrations of elements. A low-level gamma spectrometer was developed. Additional topics discussed included Optical and Electron Microscopy (X-10), Radiochemical Analyses (X-10), Reactor Projects Laboratory (Y-12), Spectrochemical and X-Ray Analyses (X-10 and Y-12), and Thermal Breeder Reactor Projects Analytical Chemistry Laboratory (Y- 12). For preceeding period see ORNL-2866.

• Research Organization: Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
• DOE Contract Number: W-7405-ENG-26
• NSA Number: NSA-15-010839
• OSTI ID: 4093642
• Report Number(s): ORNL-3060
• Resource Relation: Other Information: Orig. Receipt Date: 31-DEC-61
• Country of Publication: United States
• Language: English

Related Subjects

CHEMISTRY
ABSORPTION
ACTINIDES
ACTIVATION ANALYSIS
ALKALI METALS
ALKYL RADICALS
ALPHA DETECTION
AMINES
BERYLLIUM
BORON FLUORIDES
BREEDING
BROMATES
CADMIUM 108
CALCIUM CHLORIDES
CAPTURE
CERAMICS
CHEMICAL REACTIONS
CHROMATOGRAPHY
CONTROL
CORROSION
COULOMETRY
COUNTERS
CROSS SECTIONS
DECOMPOSITION
DELAYED NEUTRONS
DEUTERIUM
DYES
DYSPROSIUM
ELECTRIC POTENTIAL
ELECTROCHEMISTRY
ELECTRON MICROSCOPY
ELEMENTS
ETHYL RADICALS
FABRICATION
FILMS
FISSION PRODUCTS
FLUORIDES
FLUORINATION
GAMMA RADIATION
GAMMA SPECTROMETERS
GASES
GOLD 197
GRANITES
HELIUM
HEXYL RADICALS
HIGH TEMPERATURE
HYPERFINE STRUCTURE
INSTRUMENTS
ION RE