The semimicro determination of the methoxyl content of wood was studied, and a method for this determination was developed. The wood samples used in this study were 20-mesh powders of red pine and cedar, the sulfur contents of which were very small or negligible.
The procedure developed is similar in principle to Tappi methods, and the apparatus employed is a modification of the one designed by Neumann for micro methoxyl determination. In the present method, about 10-30 mg. of wood powder is heated with 2 m
l. of hydriodic acid (b.p. 126-127°C) for 40 min. and the reaction mixture is then allowed to cool to room temperature in 20 min. During the heating and cooling periods, carbon dioxide or nitrogen gas is passed through the apparatus at a rate of 20-30 m
l./min. The distillate is collected in an absorption trap (contg. 2 m
l. of Br-AcONa-AcOH soln.) and titrated with 0.02N-thiosulfate solution. In the above treatment, solvents (such as conventionally used) may be added to the sample. Also, scrubbers may be used, but are dispensable if the sample contains scarcely any sulfur. In all cases, however, blank tests must be conducted by employing the same amounts of reagents as used in the sample analysis. This is because blank values are so great that they cannot be ignored.
In so far as blank corrections are made, results of determination are reproducible. In experiments with wood powders, such results were obtained with or without the use of solvents and scrubbing reagents. Also, in experiments with vanillin and acetyl vanillin, the methoxyl contents thus determined agreed with the theoretical values. Choice between carbon dioxide and nitrogen gases is immaterial.
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