Die mikroanalytische Bestimmung des aktiven Wasserstoffes nach L. Tschugaeff und Th. Zerewitinoff

Soltys, Arnulf

doi:10.1007/bf02740168

Cited by 45 publications

(5 citation statements)

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“…Hochstein (58) compared his results from the hydride method in the microapparatus of Soltys (153) and in his own semimicro modification with some literature values of Grignard active hydrogen on enolizable compounds and observed consistently lower results with (he hydride, although solvent dependence was apparent with the hydride as well as with the Grignard reagent-e.g., acetophenone with lithium aluminum hydride showed 0.03 to 0.05 active hydrogen in no solvent, 0.02 to 0.03 in dibutyl ether, and 0.38 to 0.42 in dioxane. Ordinary active hydrogen compounds-alcohols, glycols, phenols, and aminesgave satisfactory results.…”

Section: Lithium Aluminum Hydridementioning

confidence: 98%

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Determination of Reactive Hydrogen in Organic Compounds

Olleman¹

1952

Anal. Chem.

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Methods for quantitatively determining reactive hydrogen in organic compounds have been reviewed to find the most suitable procedures for estimating the reactive structural units in coal degradation products. In the past, reaction with methylmagnesium iodide or lithium aluminum hydride has been used to determine total reactive hydrogen in organic compounds with an accuracy o f 1 3 to 5%. The types of compounds which have been determined are: alcohols, phenols, enols, mercaptans, acids. amines, amides, and water. Acylation methods. including acetylation, phthaloylation, benzoylation, ETHODS for quantitatively determiningreactive hydrogen in organic compounds-Le., hydrogen attached tonitrogen. oxygen, or sulfur and exceptionally reactive carbon-hydrogen structures-have been reviewed to find the most suitable procedures for estimating the reactive oxygen-and nitrogen-containing structures in coal degradation products. The chemical literature from 1927 to 1949, inclusive, has been thoroughly searched, and some earlier and more recent references have been consulted The literature previous to 1931 was reviewed by Meyer (93).Methyl Grignard reagents and lithium aluminum hydride will react quantitatively R ith reactive hydrogen atoms in organic compounds t o form methane and hydrogen, respectively. The gaa formed in each case is a memure of the "artive hydrogen." Other reagents have been reported for the determination of active hydrogen but are generally less satisfactory.Some of the active hydrogen atoms can also be replaced b i a(-yl groups, and compounds containing such hydrogen atoms are said to contain "acylatable hydrogen" or usually "acetylatable hydrogrn." ""wylatable hydrogen" and ' acetylatable hydrogen"are not strictly correct t e i m~, inaqmuch as the hydrogen is not acylated but rather replaced by an acyl group. However, these are convenient ternis which distinctly differentiate methods which involve acylation of reactive groups from the methods I T hich determine total "active hydrogen." Different reagents and conditions cause quantitative acylation of different functional groups, and consequently the terms "acylatable hydrogen" and "acetylatahle hydrogen" have little meaning unless the reagent and conditions are specified. Pa 1 Present addreas, Verona Research Center Koppers Co , Inc , Verona,formylation, and stearylation, vary greatly among themselves and give results depending on reagents and conditions. Variations of the most common method-i.e., acetylation using acetic anhydride and pyridine at approximately 100' C.-have been used to determine primary and secondary alcohols, "unhindered" phenols, and primary and secondary amines. Other acylation reagents may be advantageous if tertiary alcohols or pyrroles must be determined or selectivity of reaction is desired. Applicability of different acylation methods for determining functional groups has been tabulated.The methods of deterniining reactive hydrogen have thus been divided into two major groups-determinations of active hydrogrn and determinations o...

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Section: Lithium Aluminum Hydridementioning

confidence: 98%

“…l l a n y compounds containing active hydrogen give the calculated amount of methane when alloued to react at room temperature. A fev of t h e s e f o r example, some acids (29,153) and polymeric indoles (146)--gave high results when heated to 50' or 100" C. Roth (133), on the other hand, found that the results wereusually more quantitative at 95'.…”

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confidence: 99%

Determination of Reactive Hydrogen in Organic Compounds

Olleman¹

1952

Anal. Chem.

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“…Lieb and Schoniger (31) also suggested the use of lithium aluminum hydride for the determination of functional groups. In place of the electrometric titration proposed by the workers at the University of Wisconsin, Lieb and Schoniger make use of the apparatus of Soltys (61) for a microdetermination involving measurement of the liberated hydrogen. The procedure is a modification of the Zerewitinoff technique.…”

Section: Analytical Procedures From Scientific and Technical Literaturementioning

confidence: 99%

Essential Oils and Related Products

Guenther¹,

Langenau²

1951

Anal. Chem.

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“…Palfray, Sabetay, and Garry (86) again have suggested the use of sodamide for the determination of tertiary alcohols; the evolved ammonia is collected and determined. Naves (67) studied three well-known methods for the determination of tertiary alcohols: the method of Schyver (97) using sodamide; the method of Tschugaeff and Zerevitinov (114,115) using a Grignard reagent; and the modification of Soltys (102). Satisfactory results were obtained with the last procedure if the oils were thoroughly dried and then dissolved in benzene (or other hydrocarbon solvent) and permitted to react for 30 minutes;…”

Section: Chemistrymentioning

confidence: 99%