Table I. Iodine, rg/ml
Glucose, pg/ml
Precision Analysis CorreStandard sponding deviation, deviation, pg/ml trans.
4.0 7.94 0.04 0.1 0.2 0.5 1 .o 1.5
zt0.4 f O .3 Zko. 3 f O .3 f0.4 ZkO. 3 f 0 ,3 f0.4
Per cent deviation
zt0.05 f 0 .1 10.005 f0.004 f0.004 10.036 f0.034 zt0.036
1.3 1.3 12.5 4.0 2.0 7.2 3.4 2.3
aldehydes, acids, and ketones; and 1,2-diketones. Therefore, none of these compounds may be present in determining glucose by this method. The use of borate as a buffer may interfere with the periodate oxidation of sugars (8). Overoxidation (the consumption of more periodate by glucose oxidation than theoretically possible) is reported in the literature as a possible complication (6, 7, 9). However, analytical determinations are possible if the conditions used are kept constant. Determination of Jodine and Glucose. Typical transmittance-iodine concentration plots a t 505 and 484 m p are shown in Figure 1. (8) D. Hutson and H. Weigel, J . Chern. Soc., 1961, 1546. (9) G . Head, Nature, 165,236 (1950).
P!ots of the glucose concentration studies are shown in Cigure 2. The conditions were the same except for the differing temperature and time of the oxidation reaction. Two samples of known concentration are necessary to establish a reference line for each series of determinations. A precision analysis of typical iodine and glucose concentration-absorption studies a t 505 mp is shown in Table I. Four determinations were made for each concentration. Determinations a t 484 m p were less precise with the standard deviations being about three times greater for both iodine and glucose. The precision for the more complex glucose determination is the same as for the iodine determination. This method of iodine determination has extended Harlay’s method from a concentration range of 30 to 150 pg/ml of solution to between 4 and 10 pg/ml with good precision and accuracy. The application of this method for glucose determinations is useful for concentrations between 0.5 to 1.5 pg/ml of solution. Estimations are possible down to 0.1 pg/ml.
ACKNOWLEDGMENT The authors gratefully acknowledge the technical assistance of Russel Schmidt. RECEIVED for review November 14, 1966. Accepted March 16, 1967. This work was partially supported by a NSF Cooperative Graduate Fellowship and a NSF Summer Fellowship for Teaching Assistants.
Anion Exchange Separation and Spectrophotometric Determination of Titanium in Uranium-Plutonium Ternary Alloys Harold B. Evans and Rozetta R. Hallcock Argonne National Laboratory, Argonne, Ill. 60439 AN EXAMINATIONof the published literature on plutonium and plutonium alloys ( I , 2) covering the period through 1965 discloses only one published procedure dealing specifically with the analysis of titanium in plutonium nuclear alloys (3). Because titanium continues to find wide application in the nuclear field because of its beneficial metallurgical and nuclear properties, it was desirable to find new techniques which could be easily adapted to routine glove-box operations. The method proposed for the present application depends on the quantitative retention of plutonium and uranium o n the resin column while the titanium passes through in the eluate where it is determined spectrophotometrically as the peroxy complex. The procedure now available (3) is based essentially on the precipitation of plutonium peroxide. The method is timeconsuming, has numerous centrifugation steps, and is plagued by gas evolution and the attendant controlled conditions E. A. Cernak, Pratt and Whitney Aircraft Division, MiddleConn.. CNLM-1802-3 (1959). .2; :6. i3. Evans and J . 0. Karttunen, CSAEC Repor! ANL-6956
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