Investigation of the reaction products of 5-amino-1,3-disubstituted-pyrazoles with aromatic aldehydes. synthesis of new fluorinated 1,3,4-trisubstituted-4H-pyrazolo[3,4-e][1,4]thiazepin-7-ones

The condensation products of 5-amino-1,3-disubstituted-pyrazoles with aromatic aldehydes were identified as 2,4-dihydro-2,5-diphenyl-4-(phenylmethylene)-3H-pyrazol-5-imine derivatives Treatment of these products with mercaptoacetic acid gave new fluorine containing 1H-pyrazolo[3,4-e][1,4]thiazepin-7-ones.     

2-Nitrodiphenylamine as a versatile high-potential reversible oxidation-reduction indicator

The use of 2-nitrodiphenylamine as a reversible indicator has been investigated in the titration of iron(II) with cerium(IV) sulphate, potassium dichromate and sodium vanadate in sulphuric acid media. Accurate results can be obtained with cerium(IV) sulphate in 0.5–5.0 M acid, with potassium dichromate in 5.0–7.0 M acid, and with sodium vanadate in 5.0–7.5 M acid. With cerium(IV) sulphate the titrations are preferably conducted in 2.0 M sulphuric acid or in a 1.0 M. sulphuric acid-1.0 M pechloric acid medium. Tungstic acid, acetic acid, arsenic(III) and manganese(II) do not interfere. In titrations of iron(II) with dichromate and vanadate, the colour changes at the end-point are much more vivid with 2-nitrodiphenylamine than with ferroin.     

Synthesis of 1-(5-phenyl-2H-tetrazol-2-ylacetyl)-4-substituted thiosemicarbazides as possible antiinflammatory agents

A series of 1-(5-phenyl-2H-tetrazol-2-ylacetyl)-4-substituted thiosemicarbazids were prepared as possible antiinflammatory agents. Their antiproteolytic activity was reported.     

A new spot test for cerium(IV)

Summary A new colour reaction for the detection of cerram(IV) which can be carried out both in a test tube and on a spot plate has been described. The test solution is treated with methylene blue in nitric acid solution (11) to form a rose-red colour. This simple procedure has an advantage over the existing tests in that it is applicable in the presence of oxidising agents like chromium(VI), vanadium(V), nitrate, perchlorate and of coloured ions like copper(II), cobalt(II), nickel(II), chromium(III), iron(III), vanadium(IV), uranium(VI).

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Zusammenfassung Eine neue, sowohl in der Eprouvette wie auf der Tüpfelplatte ausführbare Farbreaktion zum Nachweis von Cer(IV) wurde angegeben. Die Probelösung wird mit salpetersaurer Methylenblaulösung behandelt und gibt eine rosarote Färbung. Die Reaktion hat gegenüber bekannten Tests den Vorteil, in Gegenwart von Oxydationsmitteln wie Cr(VI), V(V), NO₃ ^–, ClO₄ ^– bzw. in Anwesenheit gefärbter Ionen wie Cu(II), Co(II), Ni(II), Cr(III), Fe(III), V(IV) oder U(VI) anwendbar zu sein.

     

Phthalocyanines as oxidation-reduction indicators

Summary Copper phthalocyanine tetrasulphonic acid has been found to work satisfactorily as an inside indicator in the cerimetric titration of hydro-quinone and metol. It has the advantage that the indicator correction in titrations with 0.01 N solutions of ceric sulphate is much less than with the ferroin indicator, amounting to only 0.02 ml for two drops of the indicator solution.Part II: See Z. analyt. Chem. 163, 1 (1958).     

Electroweak tests with τ leptons at LEP

We report on two sensitive tests of lepton universality carried out by the 4 LEP experiments at the Z⁰ pole. From measurements of the τ polarization in e⁺ e^?→τ ⁺ τ ^?, the ratios of the vector and axial vector coupling constants of the electron and the tau lepton to the weak neutral current are obtained to beg _{v e} /g _{a e} =0.066±0.015 andg _{V τ} /g _{A τ} =0.070±0.009 respectively. From measurement of the τ lifetime and the τ leptonic branching ratios, the ratio of the coupling constants describing weak leptonic decays of the τ and the μ is measured to beG _τ /G _μ =0.996±0.008.     

Titrimetric determination of vanadium(V) and chromium(VI) alone and in mixtures with hydrazine sulphate in phosphoric acid media

Hydrazine sulphate is proposed as a primary standard reagent for the direct titrimetric determination of vanadium(V) and chromium(VI) alone and in mixtures with potentiometric and photometric end-points, in 9–12 M phosphoric acid medium. The methods proposed possess advantages over those currently available. The use of phosphoric acid as a reaction medium not only accelerates the hydrazine-vanadium(V) reaction very much but also makes it follow an accurate stoichiometric path.     

A new oxidimetric reagent: potassium dichromate in a strong phosphoric acid medium—I Titrimetr1c determination of manganese

A new method has been developed for the direct titrimetric determination of manganese^II, depending on its oxidation to manganese^III with potassium dichromate at room temperature in a strong phosphoric acid medium using a potentiometric or photometric endpoint. Oxygen of the air does not interfere. The potentiometric method gives results to an accuracy within ± 0.3% for 20–150 mg of manganese/50 ml of titration solution; with the photometric method 5–17 mg of manganese/40 ml of titration solution can be determined with an error of 0.3–1.0% depending on the amount present. Potassium dichromate in 12.0M phosphoric acid has a formal redox potential of about 1.5 V and this reagent appears to have great possibilities in titrimetric analysis.     

Analytical applications of the photochemical action of light: Determination of oxalic acid by photo-oxidation in the presence of ferric salts

A new method has been developed for the determination of oxalic acid. This depends upon the photochemical oxidation of oxalic acid in. the presence of ferric sulphate. The method involves exposing a measured volume of oxalic acid solution, with an excess of ferric alum and some sulphuric acid,tosunlight in quartz or pyrex beaker for 15 to 30 minutes. The progress of the reaction is indicated by the disappearance of the yellow colour of the ferricoxalate complex from the solution. After completion of the reaction, the ferrous salt formed is determined using standard sodium vanadate and either diphenylbenXXXdine or diphenylamme-sulphonate as internal indicator in the presence of sufficient phosphoric acid. Formic acid does not interfere in the photochemical method of deteminination.