A method of rapid determination for indium, nickel and copper in Spinach (NBS; SRM-1570) by substoichiometric radioactivation
analysis is described. The method is based on the principle that an equal amount of non-irradiated test sample is added to
the irradiated standard sample and subsequent substoichiometric extraction for the irradiated test and standard samples is
carried out. Indium is extracted as diethyldithiocarbamate into carbon tetrachloride, nickel as dimethylglyoximate into chloroform
and copper as dithizonate into carbon tetrachloride. The radioactivities of these extracts are measured by NaI(Tl) or Ge(Li)
detector coupled with pulse-height analyser. The analytical results obtained by the method were in good agreement with our
published values and certified values by NBS.
Substoichiometric isotope dilution analysis has been applied for the determination of trace elements in liquid samples, of
carrier content in radioisotope solution and of concentration of organic reagent. Cu in mineral acids and in ZnSe single crystal
was determined by the substoichiometric extraction with dithizone. The values of 1.8 and 0.018 ppm in nitric acid and distilled
one and of 1.4 and 0.44 ppm in ZnSe were obtained. Cu and P carrier contents in64Cu and32P solutions were determined by the substoichiometric extractions with dithizone in CCl4 and with molybdic acid into MIBK in the series of the solutions adding various amounts of Cu or P carrier. An analogous method
has been applied for the determination of dithizone and diethyldithiocarbamate solutions. The method was also applied for
the determination of60Co radioactivity in environmental samples. The analytical result of water samples is described.
Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were
determined by INAA. The contents of impurities in ultra-pure materials are less than those of high-purity materials and of
G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in
the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference
materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and
in four Japanese biological standard reference materials: Tea Leaves B&C, Pepperbush and Shark Meat. The analytical results
in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS.
The paper describes a method of radioactivation analysis for the determination of indium, copper and nickel. In the determination
of indium, ordinary and displacement substoichiometries were applied for glassmaking materials while ordinary substoichiometry
was applied for NBS standard reference materials. Copper and nickel in glassmaking materials and NBS standard reference materials
were also determined by the displacement and ordinary substoichiometries. Indium contents in glassmaking materials by the
two methods agreed with each other. The analytical results of indium, copper and nickel in NBS' SRM were also in good agreement
with published values and certified values by NBS.
The determination of trace elements in highly activated matrix components was carried out by neutron activation analysis using the radioisotope addition technique. The method is based on the addition to the irradiated test sample of a radioisotope which is a diffeent nuclide of the element to be determined. After separation, the chemical yield is calculated from the radioactivity added and the element is determined by an ordinary technique. Twelve elements in indium phosphide and eight elements in gallium arsenide could be determined by the method.
The cross sections of both thermal neutron capture and the (n, 2n) reaction for231Pa target have been determined by using gamma-ray and alpha-ray spectrometric methods following irradiation with neutrons possessing purely thermalized and fission-type reactor spectrum, respectively. Prior to the irradiation, a pre-chemical purification was applied to ensure the accurate determination of the target nuclide,231Pa. For the sake of alpha-spectrometric determination of the daughter230U, decayed out from parent230Pa, the chemical purification of uranium was also applied to the alpha-source preparation from the reactor-irradiated231Pa. The activity ratio of230U to232U was converted to an initial formation ratio of230Pa to232U and followed by an evaluation of cross section. The cross section value for the231Pa (n,)232Pa reaction process was estimated to be 186±13 barn for purely thermal neutrons. The231Pa(n, 2n)230Pa cross section value is 4.12±0.32 mbarn for fission type neutrons.
Trace amounts of transition elements (Fe, Co, Ni and Cu) in zirconium fluoride and NBS SRM's were determined by substoichiometric radioactivation analysis. The contents of impurities in sublimed sample were less than those of high-purity material and of reagent grade. The detection limits of these elements in zirconium fluoride were 10 ng/g for iron, 0.01 ng/g for cobalt, 1 ng/g for nickel and 0.1 ng/g for copper. The analytical results for iron, cobalt, nickel and copper in NBS SRM's were in good agreement with certified values.
The separation of fluorine was studied by several inorganic ion exchangers. A high yield of adsorption for fluorine was obtained
using hydrated tin dioxide in 1N nitric acid. Fluorosilicate can be separated under the same conditions. It was also found
that fluorine and fluorosilicate could be separated substoichiometrically. The substoichiometric separation was applied to
the determination of oxygen in silicon crystals by radioactivation analysis. The concentration of oxygen was 28 ppm and agreed
with that from a non-destructive method.
Distillation and substoichimetric precipitation for silicon have been developed for the determination of trace amounts of silicon. It is based on substoichiometric precipitation as barium fluorosilicate and the distillation of silicon tetrafluoride. The separation has been applied for the determination of silicon in gallium arsenide and NBS steel as standard reference material.
Distillation of fluoride as fluorosilicic acid and substoichiometric precipitation as lanthanum fluoride was studied for the determination of oxygen in gallium arsenide by3He activation analysis. Fluoride could be separated substoichiometrically with a good reproducibility by two distillations and successive precipitation with lanthanum. The oxygen concentration in gallium arsenide prepared by the horizontal Bridgman technique was 10 to 36 ppb and increased a little along the front, middle and tail portions in the crystal.