Abstract
In the present paper the author discusses the methods for determining total ashes of drugs. The methods from various Pharmacopoeias, abridgements and other literary contributions are compared. The author points out specially the difficulties of incinerating the drugs in certain cases, the inconveniences as to the number of operations, and the long time taken up by every determination. He relates the method from the German Pharmacopoeia VI, which uses washed and calcinated sand to facilitate the combustion. He then indicates a simplification of this method which can be executed in a muffle, on a Bunsen burner or similar apparatus. The deciding factor in choosing the present method was the speed of combustion and true incineration. By this modified method, 90 determinations of total ashes were executed on 9 lots of drugs, 10 determinations on every lot, 5 of these in a muffle and 5 on a Teclu burner. In all the cases the drug was air-dried and the results were calculated on this basis. Having described and commented on the many factors, which can influence the results of total ashes, the author maintains that the cited results cannot be compared with those found by other authors. This is due to the fact that the drugs used were not in a satisfactory condition, (see remarks in the above table), but were employed to ascertain the constancy of the results, i. e., to prove the value of this experimental method. The average values obtained in the muffle were slightly inferior to those obtained by incinerating on a Teclu burner. Only lot n. 6 gave in the muffle a mean value, 0.4% higher than on .the Teclu burner. This variation can be attributed to the use in the muffle, of the lowest and final part of the drug. The difference between the highest and lowest result in every series of 5 determinations of the same drug was always lower than 1 %, both, for the muffle and the Teclu burner. The author considers that the results obtained, are very good, concluding by the following advantages and recommendations:
1) The combustion of the drug mixed with sand is greatly facilitated by the following factors: a) Uniform distribution of the drug particles to be incinerated; b) Uniform distribution of heat; c) Air penetrating easily the central and lower portions (through temporary removal from the muffle or burner); 2) The use of white sand facilitates greatly the perception of the endpoint of the incineration, and any unburned carbon;
3) The same sand may be used for up to 5 analyses. A treatment with acid, subsequent washing with water and calcination, leave it in a perfect state to be used again; 4) The carbonization-time is greatly reduced, (average: 5 min.); 5) The true incineration-time is greatly reduced, (average : 30-45 min., in a muffle or on a gas burner); 6) The method gives very good results, for the routine, but it needs perfect homogenization of the sample, before weighing out.
References
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Copyright (c) 1953 Instituto Adolfo Lutz Journal
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