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Hygroscopic substances in microanalysis

Part II. New techniques for drying and weighing liquids, applicable to micro preparative work


Since very little was known about the drying of hygroscopic liquids for micro elementary analysis, various techniques were tested. Six drying procedures are described, compared and graded according to the amounts of sample available, direct contact with drying agents, complete separation of drying medium and liquid, and specific properties of the liquid compounds, such as hygroscopicity, vapor pressure, and viscosity.

A simple but efficient technique for the automatic filling of weighing capillaries with nearly complete exclusion of atmospheric moisture was developed.

In order to compare the efficiency of the various drying procedures, 5 to 10% by weight of water was added to organic liquids of known purity, and then removed by the appropriate technique. A fractional sample of the final product was analysed for carbon and hydrogen or nitrogen, by means of micromethods, and the percentages obtained were compared with the percentages found on the original, dry sample.

In connection with the work on the drying procedures a study was made of the factors which lead to loss of material in these manipulations, particularly losses due to evaporation, surface attraction, and adsorption. The investigation arose from a comparative study of various decigram, centigram and milligram procedures for micro preparative work.

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Alber, H.K. Hygroscopic substances in microanalysis. Mikrochemie 25, 167–181 (1938).

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