References
In our hands the most successful methods for the preparation of these compounds were as follows. Dithionates,Gay-Lussac andWelter, Ann. Chim. Phys.,10, 312 (1819).
Trithionates — Tetrathionates,A. Kurtenacker andMatejka, Ztschr. anorgan. Chem.,193, 367 (1930).
Pentathionates,Foerster andCentner, Ztschr. anorgan. Chem.,157, 80 (1926).
Behrens-Kley. Mikrochemische Analyse, 3 Auf., 237.
Emich-Lehrbuch d. Mikrochemie, 2. Aufl., pp. 139, 179.
Chamot andMason, Handbook of Chemical Microscopy, Vol. II, pp. 321–335.
E. M. Chamot andMason, op. cit., pp. 288–294.
This reagent is satisfactorily made from Benzyl chloride and Thiourea by the method ofBernthsen andKlinger, B.,12, 574 (1879). The reagent exists in two modifications, a stable form melting at 144°C. which solidifies to a metastable form melting at 175°C. Recrystallization of the product melting at 144°, gives the same two modifications. The hydrochloride crystallized from water upon an object slide yields thin rhombs and tablets whose acute angles are 74°. If however free hydrochloric acid is present curious plates and prisms are obtained with very characteristic twins so oriented as to exhibit a reentrant angle.
This reagent can be prepared by adding Ethylene diamine to an aqueous solution of Ni(NO3)2 (1 gram in 5 cc) until the solution acquires a violet color. It was proposed by Spacu and Spacu, Ztschr. analyt. Chem.,89, 192 (1932) as specific reaction for S2O3. We find that it also gives a reaction with S2O6— but with no other anions of the Sulfur Group.
F. Demöff, Dissertation, Hannover, 1923, 49.
Kley has shown (Behrens-Kley), Mikrochemische Analyse, p. 139, that Cobalt Ammine Chloride gives a characteristic reaction with pyrophosphates, by which they can be distinguished from other members of the Phosphorus Group of anions. After a few minutes standing regular hexagons and skeletons of hexagons are formed. As the test drop concentrates through spontaneous evaporation it becomes filled with a mass of hexagonal scales, plates and tablets and skeleton crystals in the form of rosettes and six armed stars.
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Chamot, E.M., Brickenkamp, R.W. Microscopic chemical reactions of some of the polythionic acids. Mikrochemie 16, 121–132 (1935). https://doi.org/10.1007/BF02740464
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DOI: https://doi.org/10.1007/BF02740464