ANALYTICAL CHEMISTRY DIVISION QUARTERLY PROGRESS REPORT FOR PERIOD ENDING MARCH 26, 1951
: 8 9 : ; 7 D 6 4 K 9 P and Fe with ceric sulfate has been effected satisfactorily at 60 deg C. Submicrogram quantities of U(VI) were isolated by filter paper partition chromatography using 2- methyltetrahydrofurane containing aqueous HNO/sub 3/ as the mobile liquid phase. The possibility of separating U(VI) from other cations by this technique is suggested. The use of radioautography and alpha -counting methods gave a highly sensitive method for locating solute sorption bands on the chromatograms. Use of the recording polarograph provided with the curve follower'' was extended to determine U(VI) at concentrations of 0.5 and 1.0 mu g/ml in 0.1M HNO//sub 3/; trace quantities of Pb in blood, urine, and air; 0.02 and 0.04 mu g/ml of In, a special technique being required to overcome difficuities in the potential region of the electrocapillary zeros and In in In--Th alloy. A special protective hood is illustrated which facilitates Pu titrations. Studies of Cr/sup 51/ decay have shown very little BETA /sup -/ or e/sup -/, and the presence of two gamma rays of 0.33 and 0.27 Mev in the ratio 3 to 1. gamma radiation was found to accompany 15% of the total disintegration, decay thus appearing to be 11.3% through the 0.33-Mev level, 3.8% through the 0.27-Mev level, and 85% directly to the ground state. A value for the half life of 27 plus or minus 0.4 days was indicated. Decay studies on Sr/sup 85/ indicated that the radiation was composed entirely of Rb x rays and gamma radiation of 0.52 Mev. The activity due to conversion of electrons appeared to be of the order of 0.2%. The decay was 77% directly to the ground state and 23% accompanied by the 0.5-Mev gamma ray. Two methods are suggested for the routine assay of low-level liquid wastes (10/sup -3/ to 10/sup -5/ mu c/ml). Dishes of four designs have been studied to repiace those in current routine use as sample mounts for gross BETA counts. A method for the separation of Am and Cm from the rare earths is being studied which consists in extracting them from an aqueous phase of pH 5 with 0.5M TTA-xylene and then stripping'' the organic phase with versene. The effect of pH on the selectivity of Am stripping is shown. A rapid method of removing deposited oxide layers or films from stainless steel was developed. The nbutyl bromide method has been found to be a suitable replacement for the Pepkowitz and Judd method for determining O in Na. Study of Dow Corning Silicone Oil 550 indicated instability at temperatures above 1200 because of polymerization, even when not in contact with Na. A gravimetric perchlorate method was developed for determining K in the Na--K-U fluoride eutectic. The pyrohydrolysis method for the determination of fluoride in ZrF/sub 4/, UF/sub 4/, ThF/sub 4/, HfF/sub 4/, and BeF/sub 2/ is recommended as an improvement over the Willard and Winter steam-distillation method. Fractional distillation of the chlorides of Ti, Nb, and Ta was investigated; the study of various chlorinating agents, resulting in the selection of heptachloropropane, is reported. NbCl/sub 5/ was almost quantitatively recovered in the higher boiling fraction. Analytical problems of the HRE are ddscussed. The ultraviolet spectrophotometric absorption method for the determination of phthalate ion In recycle liquors from the Zr refining process was shown to be sufficiently accurate for routine use. A sample of bonded graphite (Carbate) was bombarded with electrons. A microcombustion technique showed the bombardment to have effected a decrease in the H content. The synthesis of iodoacetylene is reported. (W.L.H.) Progress is reported on the following studies: ionic analysis (derivative polarography, vibrating-reed electrometer, high-impedance preamplifier, polarographic determination of Pb and Zn in Th, conductivity bridge, vacuum-fusion analysis of C --Th alloys for O/sub 2/ and N/sub 2/, potentiometric microtitrator); radiochemical analysis
- Research Organization:
- Oak Ridge National Lab., Tenn.
- DOE Contract Number:
- W-7405-ENG-26
- NSA Number:
- NSA-12-008318
- OSTI ID:
- 4343138
- Report Number(s):
- ORNL-1088(Del.)
- Resource Relation:
- Other Information: Decl. with deletions Feb. 20, 1957. Orig. Receipt Date: 31-DEC-58
- Country of Publication:
- United States
- Language:
- English
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