ANALYTICAL CHEMISTRY DIVISION ANNUAL PROGRESS REPORT FOR PERIOD ENDING DECEMBER 31, 1957
1 6 : 3 6 3 2 4 5 6 3 6 7 3with spectrophotometric studies of Pu in sulfate systems, determination of Pu/sup 3+/ and Pu/sup 4+/ in PuF/sub 3/-PuF/sub 4/ mixtures in fused NaF-BeF/sub 2/, coulometric reduction of KTcO/sub 4/, fractionation of Amsco 125-82, chemical changes occurring in UO/sub 2/-At fuel element fabrication, analysis of yttrium alloys, pelarography of Nb in citric acid, spectrophotometric determination of Nb using hydroquinone, and instrumental methods for Ni and Cr in fluoride salts for use in the High-Radiation-Level Analytical Facility. Also an enthalpymetric determination of free acid in presence of certain hydrolyzable ions was developed, and analysis of gaseous nitrogen oxides was studied spectrophotometrically. In the InLine Instrumentation Program development and testing is reported on: an interface-level controller for use with conductivity- type digital probe, an a-c polarograph for U losses in raffinate streams, a gamma activity monitor, an r-f monitor for HNO/sub 3/ in feed streams, flowrate meters, a potentiometric Cl/sup -/ monitor for Darex Process, continuous alpha monitors, densimeters and flow colorimeter. Instrumenis developed and being developed by the Analytical Instrumentation Group includei a flame spectrophotometer, a simplified controlledpotential coulometric titrator, a gamma absorption photometer for determination of U and Pu in pure solutions, an automatic spectrophotometric titrator, a buret for enthalpy titrations, and a controlled- potential and derivative polarograph. Radiochemical Analyses. Electromagnetic radiation from Pu isotopes and L-shell fluorescence yields of several nuclides were studied. Other studies of interference in alpha counting by lowenergy beta radiation, applications of gamma spectrometry, and analysis of noble gas mixtures for radionuclides are reported. Activation Analyses. Neutron activation analysis was applied to determination of microgram and submicrogram amounts of many elements in various samples. Its application in particlesize-distribution analysis is discussed. Mass Spectrometry. Design and construction of a 60-, 6- in. instrument capable of simultaneous collection of 2 neighboring isotopes of mass as low as 20 is described. Enrichment of Ar/sup 36/, Kr/sup 56/, Kr/sup 84/ , Kr/sup 80/ and Kr/sup 78/ by t hermal diffusinn is reported. Spectrochemical and X-Ray Analyses. Studies of separation of rare earths from Al and collection of rare earths, W, Ta, Nb, and Sb by chemical means are reported. An x-ray fluorescence procedure for analysis of U- Zr- Nb was developed. The spectrographic limit of detection of Li and Cs were lowered using alcohols as solvents. Inorganic Preparations. Work continued on anhydrous transition metal halides, fused salts for solvent systems, and hexahalorhenates. Optical and Electron Microscopy. Research is reported on: ThO/sub 2/ slurry program, dispersion of agglomerated, friable particles for electron microscopy, eifect of Van de Graaff generator exposure on oxide films on Zircaloy-2, 347 stainless steel, and Ti, nonconductivity of In films on Ge single crystals, and other corrosion product and surface studies. Research and development at Y-12 site continued with the HRP Analytical Chemistry Laboratory working on the improvement of methods for corrosion products in UO/sub 2/SO/sub 4/ solutions and ThO/sub 2/ slurries. Methods developed or investigated are: Zn by derivative polarograph, Ce by redox titration, As by colorimetry, Ru by flame photometry, and separation of Ru from UO/sub 2/SO/subn 4/ by pyrolysis. For ThO/sub 2/ analysis these methods were developed: Mo by colorimetry as quercetin complex, Co by colorimetry as 1-(2-pyridylazo)-2-naphthol (PAN) complex, Ti by spectrophotometry using Tiron, Al separation by
- Research Organization:
- Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
- DOE Contract Number:
- W-7405-ENG-26
- NSA Number:
- NSA-12-009686
- OSTI ID:
- 4309521
- Report Number(s):
- ORNL-2453
- Resource Relation:
- Other Information: Orig. Receipt Date: 31-DEC-58
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ACIDS- CHROMIUM- CITRIC ACID- DIGITAL SYSTEMS- ELECTRIC CONDUCTIVITY- ENTHALPY- FLUORIDES- GASES- HYDROLYSIS- INSTRUMENTS- LABORATORY EQUIPMENT- LOSSES- MEASURED VALUES- NICKEL- NITROGEN OXIDES- QUINONES- RADIATION DOSES- RADIATION EFFECTS- TESTING- THERMODYNAMICS- URANIUM
ACTIVATION ANALYSIS- ADSORPTION- ALPHA DECAY- CHLORINE- COLOR- COMBUSTION- COUNTERS- DAREX PROCESS- DENSITY- ELECTRIC METERS- ELECTRIC POTENTIAL- ELECTROMAGNETISM- FLOWMETERS- FLUORESCENCE- GAMMA RADIATION- IONS- ISOTOPES- MEASURED VALUES- MONITORING- NITRIC ACID- NUCLEI- PHOTOMETRY- POTENTIOMETRY- QUALITATIVE ANALYSIS- RADIATION