Reported is a cell designed specifically for high speed anodic stripping analysis. Metals amenable to this technique are determined at the 1-ppb level or less within 10 min total analysis time and with a precision of 5%. The cell, which is closed at the bottom and partially open at the top, is rotated at a high rate, thus forcing the sample solution into a thin film which is then sparged of oxygen within 75 sec prior to the analysis. A stirrer of new design and rotated at 180,0 rpm is employed to assure the rapid accumulation of the amalgam. Recommendations for the kinds of waxes suitable for the impregnation of the graphite electrodes employed is given. A step and hold voltage ramp is used in stripping the amalgam and the resulting digitally recorded data are transferred onto magnetic tape for processing with a user interactive program written for the CDC-6600 computer. Two methods for purifying reagent grade KCl are offered. One involves recrystallization; the other, amalgam exchange of electroreducible impurities for aluminum ions.
A bipolar digital potentiostat based upon the principle of charge injection or extraction has been built, tested and applied to polarographic and anodic stripping analyses. It is capable of o. 01% precision.
UCRL-11604 A spectrophotometric method for the determination of palladium is presented which utilizes the absorptivity of the tetraazidopalladium (II) complex at 315 m~-t. after extraction into n-butyl alcohol and back-extraction into water. The main factors which control the color development and extraction are discussed and the effects of some common foreign ions are shown. The method offers advantages in sensitivity, color stahility, speed and accuracy. The standard deviation over the optimum range from 1.3 to 4.6 p.p.m. is 0.03 p.p.m.
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