原子吸光分析法による有機化合物中のリンの間接定量(ノート)

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Phosphorus in organic compounds was determined by atomic absorption spectrophotometry. At this moment, it is difficult to determine phosphorus directly by atomic absorption spectrophotometry. However, molybdophosphoric acid produced by the reaction of phosphoric acid with ammonium molybdate is extractable with organic solvents and hence phosphorus is capable to be determined indirectly by the measurement of the molybdenum extracted by atomic absorption spectrophotometry. Although nitrous oxideair fuels have usually been employed for the determination of molybdenum, this time an attempt was made by using an acetylene-air fuel, instead of nitrous oxideair. Measurements were made with a Hitachi Model 207 atomic absorption spectrophotometer and the working conditions are as follows: lamp current 10 mA; acetylene flow rate 4.5l/min; air flow rate 13.0l/min; slit width 0.18mm and wavelength of Mo is 3133 Å. Procedures : To 5ml of a standard phosphorous solution (5μg/ml), 5ml of 60% perchloric acid was added and the mixture was diluted to 40ml with water. To this 3ml of 10% ammonium molybdate was added and molybdophosphoric acid produced was extracted with MIBK, and the extract was washed twice with water. The MIBK was used for the measurement. According to this method, a calibration curve of phosphorus shows a linear relation up to the concentration of 2.5μg/ml. Recovery was 101.9% by the back extraction with 3 M ammonia water. Under the conditions, an ionic sample such as histamine diphosphate was dissolved in water and treated by the usual procedure, while such non-ionic samples as triphenylphosphine and pyridoxal phosphate were decomposed by boiling with concentrated sulfuric acid and concentrated nitric acid and then they are treated similarly to the ionic sample. The standard deviation was 0.200.28.
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原子吸光分析法による有機化合物中のリンの間接定量(ノート)

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