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Precise determination of plutonium by potentiometric titration.
1960
Abstracts
Section
A 123
If the acid-ahydride mixture contained some other indifferent substances 2 titrations had to be performed. The sample was dissolved in methanol and one aliquot was titrated in methanol-benzene solution. Another aliquot was diluted with water (I + 10) and titrated after 1 h with the same sodium methylate SOhtiOn in methanol. The difference between the volumes used in both cases was equivalent to the anhydride content in the sample. Ad. Hu. [396] PRECISE DETERMINATION OF PLUTONIUM BY POTENTIOMETRIC TITRATION. G. R.Waterberg and Ch. Metz. (University of California, Los Alamos Scientific 31 (1959) 1144. Lab. , Los Alamos, N.M., U.S.A.) Anal.Chem.,
Macro-amounts of Pu are quantitatively oxidized with perchloric acid; the Pu (VI) is then reduced to Pu (IV) with a very small excess of Fe (II) which is then titrated automatically with Ce(IV). Standarddeviation is about 0.02%. The influence of 26 foreign metals is investigated. Only Cr, Au, Mn, V and Pt interfere. Pt and calomel electrodes are used as the indicator electrodes. Plotting of the tension values gives better results in end-point location than titrating to a pre-set potential. Kl. Gr.
w71
AUTOMATIC DERIVATIVE POTENTIOMETRIC AND SPECTROPHOTOMETRIC TITRATIONS OF ORGANIC ACIDS. H. V. Malmstadt and D. A.Vassallo. (Dept. of Chem. and Eng. Chem. , University of Illinois, Urbana, III, U.S.A.) Anal. Chem., 31 (1959) 862. The use of various electrode systems for the derivative potentiometric indication of non-aqueous titrations of carboxylic acids, sulfonamides, imides, mercaptans and enols is described. The best results are given with the couple Pt (lO%Rh) vs. a pencil lead graphite electrode. A Sargent Malmstadt titrator is used as the recorder. Tri-n-butylammonium hydroxide is used as the titrant in about 80% benzene-20% butanol. Recorded curves of various electrode couples are given. The standard deviation for all concentrations is in the range of the reading error of the burette. Kl. Gr. [3981 APPLICATION OF THE ELECTROMETRIC CONTACT METHOD IN PAPERCHROMATOGRAPHY OF SOME ORGANIC ACIDS. B. ZapiBr and J.Platek. (Dept. of General Chemistry, Jagiellonian University, Krak6w, Poland.) Roczniki Chem. , 33 (1959) 1159. The applicability of the Kamienski micro-electrode for the detection of tartaric, citric and succinic acids on paper chromatograms was investigated. Good separation of the acids was obtained and well developed maxima at the tension changes were observed. For acids with high dissociation constants the observed tension changes were also large. The electrometric contact method allowed the detection of the acids mentioned even when they were present in very small qlantities of the order of lo-l2 mole on the active surface of the electrode (3. I4 mm ). Ad. Hu. [399 1 TITRIMETRIC ANALYSIS OF 3:5-DINITROBENZOATE DERIVATIVES. W. T. Robinson, Jr. , R. H. Cundiff, A. J. Sensabaugh and P. C. Marcunas. (Reynolds Tobacco Co., Winston-Salem, N. C., U.S. A.) Talanta, 3 (1960) 307. The neutralization equivalents of 3:5_dinitrobenzoate ester derivatives of alcohols and ethers were ascertained. In preliminary investigations the 3:5-dinitrobenzoates were titrated directly in pyridine with tetrabutylammonium hydroxide.
Abstracts
Section
A 123
If the acid-ahydride mixture contained some other indifferent substances 2 titrations had to be performed. The sample was dissolved in methanol and one aliquot was titrated in methanol-benzene solution. Another aliquot was diluted with water (I + 10) and titrated after 1 h with the same sodium methylate SOhtiOn in methanol. The difference between the volumes used in both cases was equivalent to the anhydride content in the sample. Ad. Hu. [396] PRECISE DETERMINATION OF PLUTONIUM BY POTENTIOMETRIC TITRATION. G. R.Waterberg and Ch. Metz. (University of California, Los Alamos Scientific 31 (1959) 1144. Lab. , Los Alamos, N.M., U.S.A.) Anal.Chem.,
Macro-amounts of Pu are quantitatively oxidized with perchloric acid; the Pu (VI) is then reduced to Pu (IV) with a very small excess of Fe (II) which is then titrated automatically with Ce(IV). Standarddeviation is about 0.02%. The influence of 26 foreign metals is investigated. Only Cr, Au, Mn, V and Pt interfere. Pt and calomel electrodes are used as the indicator electrodes. Plotting of the tension values gives better results in end-point location than titrating to a pre-set potential. Kl. Gr.
w71
AUTOMATIC DERIVATIVE POTENTIOMETRIC AND SPECTROPHOTOMETRIC TITRATIONS OF ORGANIC ACIDS. H. V. Malmstadt and D. A.Vassallo. (Dept. of Chem. and Eng. Chem. , University of Illinois, Urbana, III, U.S.A.) Anal. Chem., 31 (1959) 862. The use of various electrode systems for the derivative potentiometric indication of non-aqueous titrations of carboxylic acids, sulfonamides, imides, mercaptans and enols is described. The best results are given with the couple Pt (lO%Rh) vs. a pencil lead graphite electrode. A Sargent Malmstadt titrator is used as the recorder. Tri-n-butylammonium hydroxide is used as the titrant in about 80% benzene-20% butanol. Recorded curves of various electrode couples are given. The standard deviation for all concentrations is in the range of the reading error of the burette. Kl. Gr. [3981 APPLICATION OF THE ELECTROMETRIC CONTACT METHOD IN PAPERCHROMATOGRAPHY OF SOME ORGANIC ACIDS. B. ZapiBr and J.Platek. (Dept. of General Chemistry, Jagiellonian University, Krak6w, Poland.) Roczniki Chem. , 33 (1959) 1159. The applicability of the Kamienski micro-electrode for the detection of tartaric, citric and succinic acids on paper chromatograms was investigated. Good separation of the acids was obtained and well developed maxima at the tension changes were observed. For acids with high dissociation constants the observed tension changes were also large. The electrometric contact method allowed the detection of the acids mentioned even when they were present in very small qlantities of the order of lo-l2 mole on the active surface of the electrode (3. I4 mm ). Ad. Hu. [399 1 TITRIMETRIC ANALYSIS OF 3:5-DINITROBENZOATE DERIVATIVES. W. T. Robinson, Jr. , R. H. Cundiff, A. J. Sensabaugh and P. C. Marcunas. (Reynolds Tobacco Co., Winston-Salem, N. C., U.S. A.) Talanta, 3 (1960) 307. The neutralization equivalents of 3:5_dinitrobenzoate ester derivatives of alcohols and ethers were ascertained. In preliminary investigations the 3:5-dinitrobenzoates were titrated directly in pyridine with tetrabutylammonium hydroxide.