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OAK RIDGE NATIONAL LABORATORY Operated by UNION CARBIDE CORPORATION for the U.S ORNL-3537 UC-4 - Chemistry . TID-4500 (26th ed.) --TJ bv *->cT ' 3 -> ANALYTICAL CHEMISTRY DIVISION ANNUAL PROGRESS REPORT FOR PERIOD ENDING NOVEMBER 15, 1963 ,/- OAK RIDGE NATIONAL LABORATORY operated by UNION CARBIDE CORPORATION for the U.S. ATOMIC ENERGY COMMISSION DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency Thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. I compl&enen, or ursfwlnesa of the informefian contaknsd in this repert. or thot thw vrs- a) any iwfo~~iorr,sppmotus. mthnd, @ praaws disclosad in this report my nor inft5h& prirotnly owned rilhts; or . Assumes an8 tlabit4?ips with tu &he use of* ~t f0m dm- rrsulttirp bm.6u~& my informatiun, awarrzfus, tmfiod, or pro&ss disclo~din *hie tq&. hs ahove, "parsw ~EtingMI bnHolt tha Cmmirsion, 4 employw pf uu of rke bmnriss~on, or emplww ss to, -any Infotmaliuh pwrmaf ta ORN L-3537 Contract No. W-7405-eng-26 ANALYTICAL CHEMISTRY DIVISION ANNUAL PROGRESS REPORT FOR PERIOD ENDING NOVEMBER 15, 1963 M. T. Kelley, Director C. D. Susano, Associate Director DATE ISSUED OAK RIDGE NATIONAL LABORATORY ' Ook Ridge, Tennessee opwrutrrrl by UNION CARBIDE CORPORATION for the U. 5. ATOMIC ENERGY COMMISSION THIS PAGE WAS INTENTIONALLY LEFT BLANK Summary PART I. ANALYTICAL RESEARCH A dc preamplifier and an ac-to-dc converter, both having high input impedance and providing buffering to the voltage source being measured, were designed for the Non-Linear Systems, Inc.. model V35A 1. Analytical Instrumentation . digital voltmeter. The converter can serve as a standard for ac voltage measurements because of its dc calibration. Several instruments were modified for specialized The design, construction, and evaluation of the applications. Detailed design information was pro- high-sensitivity, direct-reading, linear, recording, vided for the modification of an ORNL model Q- conductometric titrator was completed. A propor- 1988 controlled-potential and derivative polarograph tional temperature controller that provides essen- for molten-salt voltammetry, and of a model Q-1988A tially stepless control of titration cell temperature for use at fast scan rates with dropping-mercury to within fO.Ol°C was designed to supplement the electrodes having drop times of +2 sec, or less. A automatic temperature-compensation circuit for high- Beckman model B spectrophotometer was modified sensitivity work. The performance of the conduc- for continuous recording of the titration of free tometric titrator on about forty different chemical fluoride ion. The time per analysis was reduced systems met, or exceeded, design criteria. from 75 to 15 min, and the precision of analysis was The controlled-potential ac polarograph was re- improved. For a fused salt application, the preci- built with a new potentiostat having improved per- sion chronopotentiometer was altered to function formance characteristics. Test runs made with a with system ground isolated from earth ground. D.M. E. on solutions that contained M ~d 2+ in Also, an improved constant-current supply was 0.1 M KC1 show that the instrument achieves' ex- incorporated in the modified instrument. cellent rejection of the double-layer charging cur- Progress in controlled-potential coulometry was rent. Other tests indicate that excellent resolution achieved with the fabrication of two ORNL model of the 1n3+ and cd2+ waves (bEIl2 = 38 mv) is 4-2564 high-sensitivity coulometric titrators, and obtained. with revision to the method that describes the A model VII high-resolution, flame spectropho- ORNL model Q-2005 electronic, controlled-potential tometer, which uses a single multiplier phototube coulometric titrator. A check-out and test proce- (EM1 type 9558QA) to cover the entire wavelength dure for the Q2564 is being written. range from 2000 to 8700 A, was designed and put Development and improvement of apparatus for into service for emission photometry. Either the remotely controlled analysis of highly radio- instantaneous or integrated flame emission inten- active samples, primarily those associated with the sities can be recorded for measurement. The unit MSRE, was continued. The aligning, crushing, and can also be used with an absorption source assem- powder-transfer devices are being used in the ORNL bly for atomic absorption work. ~i~h-~adiation-LevelAnalytical Facility for the It has been observed that it is necessary to limit remotely controlled preparation of samples obtained the initial current delivered by the potentiostat in from the Volatility Pilot Plant. A hot-cell exhaust the controlled-potential coulometric titrations of filter assembly, which can be removed and replaced any of several ionic species. The reason for a by the master-slave manipulators, was designed and positive bias at high initial current (1 to 2% for installed in the hot cell of the Building 3038 Hot uranium) is not known. A study to determine the Laboratory. cause of this error has been initiatGd. iii In controlled-potential coulometry, the reference uses several operational amplifier modules to electrode may be placed arbitrarily in any position achieve the functions necessary. The cells, fabri- in the current density gradient present in the cell. cated from graphite or metal, contain a stationary One theory of electrochemical behavior suggests polarized electrode, a counter electrode, and a that when the reference electrode is placed in a reference electrode and may have a variable, uncon- region of low current density, an error in potential trolled resistive leakage to earth ground. For the can exist in the reaction zone in the region of high uninsulated cell vessels, system ground must float current density. This error, conceivably, could with respect to earth ground. Performance tests of cause the discharge of a second ion, and thereby this voltammeter are in progress. Another con- contribute an error in analysis. A study to deter- trolled-potential instrument that will have chrono- mine the importance of reference-electrode place- potentiometric and stripping-voltammetric functions ment in controlled-potential coulometry was under- in addition to the voltammetric function is to be taken. So far, no chemical evidence for the designed. existence of a potential error, even under drastic cell conditions, has been obtained. An investigation has been completed of the 2. Chemical Analysis of Advanced Reactor Fuels. feasibility of polarography for the direct determina- tion of metal complexes in the organic phase follow- Studies in this program were concerned mainly ing solvent extractions. The ORNL model Q-1988- wit11 the controlled-potet~tial cuululrrelric Lilralion FES dc polarograph was used to produce controlled- of uranium in solutions of uranium-bearing fuels potential regular and first-derivative polarograms and on the determination of various reaction prod- of cadmium and uranium in several solvent- ucts resulting from the dissolution of uranium car- extraction systems, including those of the ion- bides and thorium carbides. association and chelate types. The average-current A coulometric cell of 15-ml capacity was de- and derivative computer circuits were modified to signed especially for use with the ORNL 4-2564 permit the use of a f'z-sec, Smoler type, vertical- high-sensitivity, controlled-potential, coulometric orifice D.M.E. and the use of scan rates up to 3 titrator; uranium in the amounts of 2.5 and 48 pg in v/min. A quantitative method for the determination a total volume of 5 ml was determined with a of microgram quantities of uranium in tri-n-octyl- relative standard deviation of 0.8 to 0.2%, respec- phosphine oxide extract was developed. Polarog- tively. raphy in the organic extracts from solvent extrac- A controlled-potential, coulometric method for . tion offers the following advantages: the substance the dctcrl~linatisi~sf ilraiiclln ill ~ulliu~lllluu~lde to be determined can be concentrated selectively, solutions was developed. At the 6-mg level, Ure matrix elements that interfere are removed, and a relative standard deviation is 0.2%. separate stripping step into an aqueous medium is Sb~dieson the determination of carbon in aqueous not required. Also, the possibility exists of per- and nitric acid solutions from the dissolution of forming polarographic analysis on species unstable carbide type fuels were continued. A gas chroma- in water. tographic measurement of the CO, produced by The compensation of cell resistance by con- oxidation of the carbon-containing compounds was trolled-potential polarography was studied. It was incorporated into the procedure to effect an im- found necessary to place the reference electrode within a distance of 0.1 r (where r is the radius of provement in sensitivity of some twentyfold over the drop) from the mercury drop in order to avoid the manometric measurement of CO,. The inter- distorted polarograms in solutions of high specific ference of residual oxides of nitrogen is also elim- resistance. An electrode apparatus consisting of a inated by use of the gas chromatographic measure- sharpened, Smoler type, vertical-orifice, '/,-sec ment. Gas chromatography was used to resolve and D.M.E. and a reference electrode probe was con- determine the products from the reaction of carbide structed for this study. fuels with CC14 in the presence of air.
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