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- Author or Editor: T. Shigematsu x
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Abstract
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.
Abstract
The simultaneous substoichiometric separation of europium and terbium is presented and its application to the determination of these elements with DTPA and HTTA is developed. Experimental results for the simultaneous substoichiometric separation are in good agreement with the theoretical results introduced by the principle. Europium and terbium in orchard leaves are determined by simultaneous substoichiometric neutron activation. The analytical values are 23±1.1 ppb for europium, and 17±1.2 ppb for terbium.
Abstract
This paper presents simultaneous substoichiometric separation of four rare earth elements; samarium, europium, terbium and ytterbium. The elements are separated simultaneously and substoichiometrically by forming their complexanates with substoichiometric DTPA and extracting their unreacted parts with HTTA. Application to the determination of these elements by substoichiometric neutron activation is also presented.
Abstract
A study of the substoichiometric extraction of phosphorus is described. Phosphorus was extracted in the form of ternary compounds such as ammonium phosphomolybdate, 8-hydroxyquinolinium phosphomolybdate, tetraphenylarsonium phosphomolybdate and tri-n-octylamine phosphomolybdate. Consequently, phosphorus was extracted substoichiometrically by the addition of a substoichiometric amount of molybdenum for all four phosphomolybdate compounds. On the other hand, phosphorus could be separated substoichiometrically with a substoichiometric amount of tetraphenylarsonium chloride or tri-n-octylamine. Stoichiometric ratios of these ternary compounds obtained substoichiometrically were 1∶12∶3 for phosphorus, molybdenum and organic reagent. Applicability of these compounds to phosphorus determination was also discussed.
Abstract
Phosphorus in orchard leaves (NBS SRM-1571) and spinach (SRM-1570) was determined by various substoichiometric analytical methods such as the direct method, GRASHCHENKO's method and the method of carrier amount variation. All samples were labelled with32P radioisotope. The data obtained by the method of carrier amount variation were also treated by the method of least squares instead of De VOE's method. Phosphorus concentration in orchard leaves was 0.206±0.011% by the direct method, 0.219±0.011% by GRASHCHENKO's method, 0.211±0.011% by the method of carrier amount variation and 0.207±0.007% by the method of least squares, respectively. These values agree with the value reported by NBS (0.21±0.01%). Furthermore, these concentrations obtained by various substoichiometric methods were compared with those by radioactivation reported in a prevoius paper.
Abstract
Substoichiometric extraction of chromium with tetraphenylarsonium chloride (TPACl), tri-n-octylamine (TNOA), diethylammonium diethyldithiocarbamate (DDDC) and ammonium pyrrolidinedithiocarbamate (APDC) was examined in detail. Chromium can be extracted substoichiometrically in a pH range, which is 1.1–2.6 for the TPACl compound, 0.6–2.3 for the TNOA compound, 5.1–6.4 for the DDCC chelate and 3.9–4.9 for the APDC chelate. Chromium in high-purity calcium carbonate, Orchard Leaves (NBS SRM-1571) and Brewers Yeast (NBS SRM-1569) was determined by neutron activation analysis combined with substoichiometric extraction by DDDC and APDC. The values of 2.0±0.02 ppm and 2.6±0.2 ppm were obtained for Brewers Yeast and Orchard Leaves, respectively. These values were in good agreement with the values reported by NBS. The reaction mechanism and the reaction ratio between hexavalent chromium and dithiocarbamate were also discussed.
Abstract
Determination of trace impurities in zinc selenide was carried out by substoichiometric neutron activation analysis. Trace impurities were separated from matrix elements by suitable procedures and determined by substoichiometric methods, i.e., Au was extracted with rhodamine-B, Ag and Cu with dithizone, Cr with sodium diethyldithiocarbamate, Co with 1-nitroso-2-naphthol, and Sb with cupferron. Two sorts of zinc selenide single crystals were supplied for analysis and the following values were obtained as impurity concentration; Au 0.36, 0.076 ppb, Ag 42, 32 ppb, Cr. 1.8, 0.63 ppm, Co 0.16, 0.0079 ppm, Sb 8.5, 5.9 ppb and Cu 1.4, 0.44 ppm. The behavior of copper by heat-treatment of zinc selenide was also studied by means of substoichiometric isotope dilution analysis.
Abstract
Methods for simultaneous determination of europium and terbium based on concentration dependent distribution is described. With these methods, the distribution ratios of elements are measured in two types of substoichiometric systems. Possibility of determining these elements simultaneously is investigated experimentally by using two pairs of substoichiometric complexans/excess extracting agents, such as DTPA/HTTA and EDTA/HTTA. Relative errors and precisions for simultaneous determination of the elements are less than 5%.
Abstract
The substoichiometric determination of some impurities in gallium arsenide and selenium supplied by OEC and IUPAC, respectively, as reference materials for radioactivation analysis is described.
Study on the comparator method using substoichiometry
II. Simultaneous multielement determination of rare earth elements
Abstract
The comparator method using substoichiometry is developed. In the method, the contents of the elements can be determined simultaneously by the measurement of radioactivities of the comparator elements and of simultaneously separated parts of the elements in question. The method is applied to the simultaneous determination of rare earth elements, such as lanthanum, europium and terbium in NBS botanical standard reference materials. It is confirmed that the method is reliable for simultaneous multielement determination.
